08-22-01 19:58
No 206580
I never saw this thread, was in neverneverland around that time, but was just attentioned to it by Post 252772 (Goodtimes: "Re: external heat for Al/Hg", Newbee Forum).
The enormous amount of sampled info from all these splattered pieces of wisdom, about the mentioned procedures, laying around in the Hive, let's me decide, even after reading Rhodium's critique, to make it a Sticky thread, leaving it open to the public, but only for those proposed corrections already mentioned by Rhodium, by serious contributors, or any interesting additions.
Moderators will then correct eventual serious mishaps in this thread, in redtext.
Any riffraff from people in need of bulk-amounts of attention will be deleted.
The members mentioned in this Project Blackbook are ofcourse invited to add their latest findings regarding streamlining their procedures. LT/
Well everybody...here it is. This is my personal file chak full of notes that I've made over the past year and a half on anything pertinent to the process of going from sas oil to mdma.hcl via the Wacker oxidation and methanol aluminum-mercury amalgum amination.
I've cleaned the file up a bit...have taken out all references to sensitive sources and most repeated information, but not all. If anyone would like to review this file and suggest any changes or additions, I'm all for it. And if any misinformation is anywhere in here I'd especially like for someone more astute than I to make a note of it. As an example, I've read posts of different folks suggesting using vacuum, and specifically not using vacuum when filtering a chilled post wacker rxn. So both suggestions are in my notes. Any advice not fairly valid I have deleted from this file, though. All info. herein has been gleaned from what others have written at the hive...none of it is from my own personal experiences. No shit. Tax, title, and license not included.
Just thought it was time to contribute back. Welp...happy reading!
Oh...one more thing...here's how to make a cheap and very effective smell eliminator. If you're exhausting, and I highly recommend against this practice of exhausting. I'd run my vacuum output through a bucket of activated charcoal before I put a thermographic dot outside my house. But if you are, put the device I'll describe below somewhere inline. Ozone isn't good to breathe so make sure your system is well sealed or at least make sure its operating on 100 % negative pressure. If possible, exhaust either through or next to a large window ac unit. It'll churn up the exhaust dilluting it with outside air.
Sheet both sides of any piece of glass with a maleable metal (al foil) making sure each piece of metal doesn't come closer than 1 inch to the edge of the glass.. Isolate it from other objects. Take a transformer from a neon sign and disconnect its wires from the glass tubing. Now run each of these two wires...one to each sheet of the foil on each side of the glass. Turn on the transformer...voila...lots and lots of O3. You'll know its working by the buzz sound the device makes. Make sure not to touch either of the two transformer wires singly or at the same time... touching only one shocks the piss out of you. Some suggest using a quart jar and lining it with foil on the inside and outside. Others take a plate of glass from HD, epoxy (v) metal fencing (square holes 1/4" wide)(also from HD) to either side of the plate of glass leaving a one inch boarder of glass outside the wire fence. Work the wire so that it all rests against the glass as flatly as possible. Also, the epoxy used must specifically state on the packaging that it can be used for both metal and glass applications. Not all epoxies bond to glass well. This type of a device absolutly kills pungent mj smell with lots of room to spare. How much O3 this type of device can produce is directly related to both the area of the two pieces of metal used and the the size of your neon sign transformer. As a side note, splicing a dial type fan speed regulator anywhere in the system is entirely ineffective. I've no personal experience using this device to eliminate chm. rxn. odors, but I have an idea it might be as effective.
Previously I tried to post this entire file with one press of the 'post' button but it didn't work for whatever reason. So I'll be posting this now as a series of thread entries..hopefully this won't take too many posts to accomplish. The file is about 125 kb though.
Signed, sealed, delivered...
SECTION ONE - Distilling Sassafras Oil into Safrole
1) - can add high-oleic safflower oil (all natural, no preservatives) to sas when distilling so as to
get the very last drop of safrole w/o scorching flask and burning it dry
2) - always use a teflon coated stir bar to eliminate bumping - use a strong magnet applied to
the bottom of the flask to retain stir magnet when transferring contents to another container
3) - use a vac that pulls at least 27"
4) - wrap column in insulation or a number of layers of foil (wrap claisen adapter also) -
plumber's insulation (~1" fiberglass insulation coupled with a layer of foil) is far superior
in its insulation properties than just plain aluminum foil alone.
5) - thermometer bulb (top of it) 1/4"-1/2" below bottom of side arm of dist. setup leading to
conndensor
6) - always wash receiving flask with a couple of squirts of dried acetone if discarding first
distillate fraction then using the same receiving flask to collect the 2nd or 3rd distillate
portions (the goods).
7) - always use ROUND bottom flask when vac distilling - flat bottom may implode with vacuum
8) - disconnect hose from aspirator (when removing vacuum) instead of just turning h2o off to
stop vac. Doing this will ensure no h2o suckback into the receiving flask
9) - oil bath will need to be ~30C higher than distillate coming over for successful distillation
10) - always increase temperature VERY SLOWLY
11) - when using an oil bath, expect to experience a lot of thermal lag
12) - when distilling 1-2 drops per second = ~100ml an hour
13) - should take between 4-7 hours to distill sassafras to safrole
14) - sassafras oil is usually between 80-95% safrole
15) - can collect portion coming over right under safrole's bp and reprocess with a later batch to
get the safrole out of that fraction
16) - stir bar must be spinning fast to prevent bumping. Slow spinning stir bars will evidently still
allow bumping to occur
17) - when distilling sas., safrole in receiving flask will be clear to slight yellow tint
18) - need to get oil bath oil level to come up to the level of the liquid/oil in distillation flask if
possible
19) - is good to have a stir bar in both distilling flask (a must) AND in the oil bath just below the
center of the distilling flask (can be a large paper clip)
20) - cold water through condensor - but will cause need for real good insulation up to claisen
adapter because a cool condenser transferrs its coolness down through the distillation
apparatus
21) - distill with tube leading from the aspirator down past U curve under kitchen sink (to rid air of
distillate smells)
22) - safrole bp @ 10-11 mmHg is 100-101C
at 0" vac. (no vac whatsoever) safrole comes over @ 232C
at 27" vac., safrole comes over at less than 130C
VAC (mm Hg) SAFROLE BP
90 159 C
80 155 C
70 152 C
60 148 C
50 143 C
40 137 C
30 129 C
20 120 C
10 106 C
23) - always use high vac joint grease when distilling
24) - to separate components in a matrix, they must have at least 25 C difference in their boiling
points to vac distill and separate them
25) - do not use any type of mineral oil in place of high vac joint grease - always use high vac
joint grease
26) - to distill sassafras oil you want 5-10 drops a minute when distilling all fractions
27) - a slow distillation is always achieves a more distinct separation when compared to the
freezing technique.
28) - can use heating tape to wrap components with to aid in distilling
29) - distilling flask should be no more then 1/2 - 1/3 full at beginning of distillation
30) - boil over occurs if vac suddenly varies - could be shitty vac source or a change in water
temp/pressure going through aspirator - or if vacuum pump is plugged into the same
circuit the heating plate is plugged into, the simple on/of function of the plate might be
enough to interrupt the vac pump's voltage source resulting in a rise and fall of effective
vacuum
31) - good pump that pulls 28.5" Hg - KNF Neuberger teflon head diaphram pump - 'bout $500
used
32) - digital hotplate/stirrer - Fischer 11-496-80 - $595 - and get Thermocouple Immersion probe
11-496-94 @ $120
33) - a large paper clip can be used to stir oil with instead of a stir bar - its flat so that helps keep
more of the distilling flask in the oil
34) - there is at least a 10 min. delay in increasing hot plate dial temp and seing a temp rise on
the thermometer placed just before the condensor
35) - color of safrole is water-white - this indication is better than using thermometer temp
reading to discern when the safrole is coming over
36) - insulate setup all the way up to the take off where the condensor begins
37) - good insulator ="plumbing flame/heat protector" soft cottony material less than 1" thick with
aluminum backing that resembles super heavy foil - plumbers use it to shield stuff being
whatever it is they're heating from the heat of their torch.
Brand name : Alpha Fry contact info: Fry Technology, A Cookson Company, Riviera Beach,
FL 33404
Some have said on the board that this type of insualtion (plumber's) ABSOLUTLY KICKS
ASS over regular thin tinfoil.
38) - to insulate, do this: vac grease on joint surfaces and teflon tape wrapped around outside of
joint seams
39) - MM says use no water in condensor when distilling sassafras oil to safrole...keeps
distillation apparatus too cold - can pump air through it though
40) - always use an egg-shapped stir bar and no other shapes, rods, etc.
41) - then osmium says using h2o in your condensor won't effect to a bad distillation
42) - can use DOT 5 brake fluid for an oil bath when distilling - smokes first 2-3 times used then
doesn't anytime after that - professionals use some type of silicon oil though
43) - can use a fishtank air pump and pump air through the condensor instead of h20 when
distilling sassafras oil
44) - use stainless steel bowl for hot oil bath mixture. If glass is used for this oil bath bowl and
the glass breaks, or cracks, oil will hit the heating mantle and immediatly a large lab fire
ensures...so use stainless steel bowl for oil bath that won't crack like glass might
45) - usually everything coming over before bp of safrole is reached is considered forerun
Hints On Distilling Sassafras Oil Into Safrole
1) high stirring
2) big stirbar
3) make sure there are no leaks
4) raise C slowly
5) insulate all up to condensor
6) change pump oil often
46) - 1 drop every 1-2 seconds = 150-200 ml distillate per hour
47) - need hot plate at least 500 w for distillations
48) - insulate neck and riser assemblies with foil then insulate the whole thing again in a wrap
around of foil
49) - don't distill to dryness - BLACK CRAP WILL NOT COME OUT !!!! - use high-oleic safflower
oil as a distillation buffer
50) - if using fridge pump as a vac. source, make sure to direct a high speed fan on it
continuously during operation to cool it down
51) - when distilling sassafras oil , 5% is of lower bp (water?) and 15 % of the stuff is of higher
bp...collect the middle 80%
52) Osmium has said - "when I distilled sassafras oil, there was always some water in it that
came over first when heating started, ruining the vacuum. Usually I had to dry the
condenser at least once because of all that low boiling shit, because no decent vacuum
can be achieved as long as it is inside your setup. Gasses absorbed in the sassafras
oil should be gone real quick when vacuum is applied (unlike water and other low-
boiling shit)"
SOOOOO...the lesson here is when distilling sas oil, distill without vacuum (using a
condenser) to like 130C or something just to make sure all the water and other low
boiling shit is gone from the sas oil. After this is done, cap the sas oil and let it cool
back down to room temperature before applying vacuum and distilling. It must cool down
before restarting because if vacuum is applied to hot sas oil it might start coming right
over as soon as the low vacuum is reached...or it might start boiling (bumping) violently
even with good stirring.
53) When sassafras oil is distilled, if any tar is left in the original distillation flask acetone and
a baby bottle brush gets the tar (burnt) out nicely.
54) Bee says to keep all your yellow leftovers (whats still in the distillation flask) from distilling
sassafras oil and combine it to later redistill and a good amount of sasfrol will come over.
END OF NOTE SECTION ON DISTILLING SASSAFRAS
We hold these truths to be self evident.
(Stranger)
08-22-01 20:26
No 206586
SECTION TWO - Methyl Man's MeOH p-Benzoquinone Wacker Oxidation Write-Up and Notes
Materials:
400 ml MeOh
50 ml dH2O
150 g p-benzoquinone - EXPOSE TO AIR ONLY THE SHORTEST POSSIBLE PERIOD OF TIME
WHEN REMOVING FROM STORAGE VESSEL THEN REPLACE LID ONLY AFTER PLACING
SOME SORT OF HYGROSCOPIC MATERIAL (PACKED) INSIDE DEGRADES VERY
QUICKLY ONCE EXPOSED TO AIR THEN IT WILL DEGRADE TO BROWN BEING NO
GOOD
2g PdCl2 (or 1.850g)
178g safrole
DCM (dichloro methane or methylene chloride) - 900 ml
NaCl (saturated soln. of sodium chloride (non-iodized) in dh2o)
Sodium Bicarbonate (saturated soln. of baking soda in dh2o)
NaOH (5% sodium hydroxide soln. in dh2o) ~ 150g
HCl (muriatic acid ~31.45% from pool store) need ~600ml of 31% to make 1.7L 10% HCl
MgSO4 (epsom salts for drying)
1) equip -> 2L ROUND bottom flask 24/40, addition funnel, reflux condensor
place 400 ml MeOH, 2g PdCl2 (MeOH + PdCl2) in flask and let stir (stoppered!) for 3 hrs.
2) Place 178g safrole mixed with a bit of MeOH (50 ml or so) in an addition funnel
3) Add safrole/MeOH dropwise over 60 minutes or more (while stirring). When addition is ~80%
finished, apply low heat just sufficient to start a mild reflux (cold h2o through condensor).
4) Let all this reflux while stirring for 8 hours. If stopping at this point seal well and put in freezer
as ketone decomposition will occur.
5) After refluxing for 8 hours, seal the reaction vessel and let cool to room temperature. Then,
further, place it in the freezer to chill the solution (~45F?) for the purpose of crashing out
extra hydroquinone from the solution.
Then, gravity filter soln. through coffee filters to remove remaining hydroquinone
and PdCl2 - DO NOT VACUUM FILTER this soln. as both hydroquinone and PdCl2 will be
pulled through the coffee filters
- let the soln. cool to AT LEAST room temp. before filtering
- wash filter with MeOH to push remaining ketone through
6) Flood filtered solution with 1.7 L 3N ( ~10 %) HCl
- to make 3N 10% HCl add 500 ml of 31% HCl to 1150 ml dh2o to get
1.65 L ~10% HCl which is close enough
7) Extract flooded mixture with 3 portions of DCM (1 x 500ml, 1 x 250ml, 1 x 100ml) in a large
separatory funnel. The desired raw product migrates into the DCM as an oil.
- separate all the DCM/ketone layers and combine them together with themselves
- Note: when flooded mixture is first high with DCM, a layer of scum will develop which will
float on top of the h2o layer. This scum layer will work its way down during the 3
extractions to appear as a blob of spongy semi-solid interface, but its mobile and easy
to work around. Just avoid letting it into the DCM separations. Same thing happens in
washes in steps 10, 11, and 12
- DCM is the bottom layer during these steps outlined above
- emulsion (in between layer) will disappear over time if let to sit (vibrator may be of use here)
8) Extract water layer with a final small amount of DCM (~100ml)
9) Add last (4th) 100mL DCM layer to previous 3 extractions DCM/ketone solutions.
10) Wash the ketone/DCM solution with saturated sodium bicarbonate (baking soda) in water
twice (500 ml each wash). This is done in a sep funnel.
11) Wash the ketone/DCM soln. with saturated (non-iodized) NaCl soln. 3 times (400-500 ml
each wash).
- Note: when doing the bicarb and salt water washes, the DCM/ketone layer should get
progressively more greenish colored - this should be visible in the film of solution that
runs down the inner surface of the sep. funnel.
12) Wash further the ketone/DCM soln. 3 times with 500 ml 5% NaOH (500 ml each wash for a
total of 1500 ml)
- Note: upon doing the first of these 3 NaOH washes, a very noticeable color change will
occur wherein the ketone/DCM layer becomes a strange, thick reddish-brown, almost
orange color. This happens as the NaOH pulls the majority of the solvaged hydro-
quinone into its layer, cleaning the ketone. The NaOH layer in the first wash will be a
very dark brown, almost black. The next two will be far lighter, watery, orangy color.
13) Dry ketone/DCM soln. with ~50g baked and pesteled magnesium sulfate (MgSO4)
14) Distil off the DCM using mild heat on a water bath and ICE COLD water through the
condensor. This will take several hours.
15) When DCM is distilled off, add 50 ml of high-oleic safflower oil (no additives!) to the ketone
oil as a buffer to prevent the ketone from scorching the distillation flask. (Can also take
after-run from original sassafras oil distillation which has been distilled to a higher
temperature than what safrole comes over and use this as the ketone oil buffering agent?)
16) Vacuum distil the ketone/buffer oil solution. This will also take a few hours but not as long
as distilling the DCM off does. Ketone comes over (@ same vac. pressure) 35-40 C above
what safrole come over at. NOTE here that ketone should never reach a temp of 180C under
any circumstances...vacuum or no vacuum. If ketone reaches 180C it WILL carbonize !!!!
NOTE: notes on this part of the rxn. say to expect 6-8hrs time to distill ketone.
17) At 100-140 C (depending on vacuum), a minor amount of safrole might come over. If only
a few drops to a ml or two, it can be left in. And if more than this, change receiving flasks
after the safrole comes over to a new clean flask.
18) Ketone should begin coming over 25-40 C above what temperature safrole came over at at
the same vacuum pressure. ~ 100-120 g ketone should distil over - ketone color should be
pale, florescent-looking greenish yellow - not unlike antifreeze. Stop distilling when rate of
ketone coming over is 1 drop per 90 seconds or greater. Not much ketone left to distil over
at this point.
19) Immediatly store purified ketone in the freezer in an airtight flask or bottle.
19b) Remove boiling flask of undistilled ketone from hot oil bath VERY SOON after the
distillation is complete. Because if the ketone / tar mess is left to sit in the hot oil
bath it will carbonize and will be almost impossible to clean out
DONE
END OF PROCEDURAL STEPS SECTION OF THE MM P-BENZO WACKER
Short Note version of p-benzo Wacker :
1) Add 400ml MeOH + 2.0 - 1.850g PdCl2 -> 2L RB 24/40 flask - seal - and stir for 3 hours
2) 178g safrole + 50ml MeOH -> charged into an addition funnel
3) Add safrole / MeOH dropwise over 1hr. while stirring with cold condensor
4) After addition is finished - apply heat to 70 C and reflux for 3 hours
5) Stop heating - cool solution - then gravity filter to remove PdCl2 and hydroquinone
6) Flood solution with 1.7L 10% HCl acid
7) Extract flooded mixture 4X with DCM - 500ml, 250ml, 100ml, 100ml - save and combine
bottom ketone / DCM layers
8) Wash DCM / ketone layer with sat. solution of sodium bicarbonate (baking soda) 2x w/ 500ml
9) Wash DCM / ketone layer with sat. NaCl solution 3x using 500ml each wash
10) Wash DCM / ketone layer with 5% NaOH solution 3x-5x using 500ml each wash
11) Dry DCM / ketone layer with 50g MgSO4
12) Distill DCM off with mild heat and no vacuum and COLD h2o in condensor - 3hrs.
13) Add buffer oil to resultant and vacuum distill ketone - stop when getting 1 drop per 90 sec.
14) Store purified / distilled ketone in an airtight container in the freezer
The Streamlined Benzo Wacker (by Methyl Man 8-14-2000)
same as the MeOH benzo wacker above but with these changes:
CHANGE 1) PdCl2 (only 1.850g this time ) and MeOH were prestirred for 2.5 hours.
no change 2) p-benzo + 50ml h20 added and stirred vigorously for one (1) hour.
no change 3) safrole added briskly dropwise over one (1) hour
CHANGE 4) when addition was finished, a temperature of 70 C was attained and then
maintained for a mere 3 hours
(maintaining 70 C allows for a shortened rxn. time of 3 hours whereas
8 hours of rxn. time is needed when done at 55-58 C)
yield = 121 g ketone
The above rxn. scheme cut the normal rxn. time to less than half
We hold these truths to be self evident.
(Stranger)
08-22-01 20:31
No 206587
NOTES ON THE MM BENZO - WACKER:
1) Let solution cool before filtering hyudroquinone/PdCl2 out. This helps to get out more hydro-
quinone. Leaving hydroquinone (solid or in solution) causes condensors to fill up with black
stuff during later distillations. Possibly make it a point to use small micron filter paper
instead of just coffee filters here. Just a reminder: vacuum filtering through either filter paper
or coffee filters WILL cause both solid hydroquinone and PdCl2 to come completely through
the filter paper...this is because both the quinone and pd salt are microscale solid
suspensions.
2) Expect 6-8 hours to distill ketone.
3) Don't let the ketone distillation run to near dryness. Or, the solution will carbonize shooting
black crap down into your beautiful distilled ketone in the receiving flask.
4) Blue_Diamond says: make sure stirring is hard during this rxn. Might need to kick start stir
bar by hand swirling flask at first.
- says to really give those emulsions time to settle ~ 15 minutes or so
- blue_diamond does 8 x 500 ml NaOH washes to remove all the hydroquinone instead of
just the 3 x 500 ml NaOH soln. washes as MM suggests. ANY hydroquinone not washed
out of soln. causes condensor to clog up when distilling with black crap. Maybe could
compromise here...maybe 5 NaOH washes x 500 ml
- blue_diamond says: do NaOH washes until you see a light-orange khaki color in the DCM/
ketone solution.
5) Blue_Diamond - DCM boils off @ ~ 40 C with no vacuum pressure. Will take ~ 3 hours to
boil off all the DCM. After DCM comes off (slowly so no bumping), crank heat to 80-90 C. If
up to 90 C and no black crap has appeared in the condensor then all the hydroquinone was
removed with the NaOH washes.
Blue Diamond Timeline for Methyl Man's p-Benzoquinone Wacker Oxidation Reaction
0:00 add PdCl2 and MeOH
3:00 benzoquinone and MeOH and stir
4:00 add safrole
4:45 kick start heat
5:30 safrole addition complete
11:30 turn off external heat
THIS IS A GOOD STOPPING POINT. MAKE SURE TO STORE THE KETONE SOLUTION
IN AN AIRTIGHT CONTAINER ONLY AS LONG AS OVERNIGHT
0:00 / 13:30 reaction done: start washes
4:00 / 17:30 washes done: begin DCM distillation
7:30 / 21:00 DCM done: begin vacuum distillation of ketone
11:30 / 25:00 ketone reached
16:30 / 30:00 ketone finished
6) Blue Diamond says: don't go until 1 drop every 90 seconds. when distilling the ketone -
ketone will carmalize pushing black crap into the distilled purified ketone in the receiving
flask. Start paying attention when @ 1 drop every 15 seconds and shut it down when it slows
to 1 drop every 30 seconds...will give between 90-100 ml ketone every time.
7) Bright Star says: the 2 prestirrs can be done for as long as one likes...nothing adverse will
happen if solutions are prestirred for an untraordinary long period of time...just make sure
the solutions don't evaporate when stirring (for either long OR short periods of time).
8) Bright Star says: can start heating the reaction as soon as all the safrole has been added.
But generally not before
9) Expect goopy dregs to be left in distillation flask after final ketone distillation/purification.
10) Hexane might be a future extractor to get the last ketone out of the goopy dregs left over
from the ketone distillation. Hexane = ~ $8 / Liter.
11) Methyl Man uses a 4000 mL separatory funnel when flooding post reaction mixture with
10% HCl
12) Methyl Man says: turn heat on lowest setting to reflux after 80% safrole is complete. MeOH
bp = 65 C so temp. on low setting (1-one) should be enough.
13) To make saturated wash solutions...put X mls dh2o into beaker on hotplate/stirrer and stir
vigorously. Then add solute (salt, NaOH, etc.) until its obvious no more solute dissolves.
Stir for quite a while with solids visibly still not dissolved, then filter solution.
14) When refluxing after safrole addition, column should yeild 1 drop every 4-5 seconds and NO
MORE ! If more drops falling from condensor faster than this, then the heat on the hotplate
is turned too high. Too high heat encourages iso-formation away from MD-P2P. So turn the
heat down if necessary so as to preserve product yield %.
15) Bright Star says: One of the "secrets" of this reaction is to let the PdCl2 dissolve in the
MeOH over a period of 2-3 hours.
16) Looks like solution should might even be cold when filtering out solid hydroquinone.
BUT, reports show that if TOO cold then the solid hydroquinone might stop up the filter
17) MM NOTE: When you get to that first NaOH wash, the product turns a rusty orange
color. The top layer is the NaOH / crap / hydroquinone layer and it is a vivid blackish-
reddish-brown color and looks more enviting than the bottom DCM / product layer, which
looks like a carrot juice - DCM cocktail. The point of this note...is to make sure you know
which layer is which in the seporatory funnel and DO NOT throw away the wrong layer!
18) MM NOTE: This reaction heats up on its own if the safrole is dripped in at a fast enough
rate.
19) Bright Star says: 99.99% MDP2P (double distilled) doesn't degrade at room temperature
when kept for 30 days via benzo wacker oxidation. But, ~97% MDP2P (single
distillation) degrades 21% per week.
20) Bank Robber says: to prestir MeOH / PdCl2 for 20 hours ! ... if any PdCl2 is seen
undissolved anywhere when stirring is stopped, then KEEP STIRRING!
MM confirms 132g ketone from 178g safrole when he prestirred PdCl2 in MeOH for 8
hours
21) LABTOP says - when distilling ketone - a good indication that something is coming over
(after the ketone distills) that you DON'T want "is when the first slightly yellow distillate
drops in the distillate flask and gives those yellow swirlings falling down." The rest that
comes over put with the next batch of a post reaction ketone (post washes also) to distil
and regain any post cursor ketone.
22) NaOH washes and filtering are both done for the purpose of removing hydroquinone - if
not much solid hydroquinone filters from solution, then make sure to do enough NaOH
washes later to get it all out.
23) Methyl Man -> After bicarbonate and NaCl washes, the wash water should be getting very
pale.
24) Of course - cover beakers during 20 hour (or any length) prestirring.
25) If pre-flood filtration isn't done to remove solid hydroquinone, the first NaOH wash causes
2 black layers not discernable from one another...BAD ... One way to discern two
indistinguishable layers is to turn out the room lights and to shine a flash light on the
layers...this might / should show the two layers as separate. Another way is to use a
black light (lab grade lambda) (light or dark room?) to discern the two layers.
26) When distilling ketone, put either a large paper clip or stir bar in the oil bath to ensure
proper temperature distribution in the oil or water bath and that no hot spots occur.
27) One can freezer chill the DCM / oil / quinone mix before filtering but must vacuum filter if
the solution is this cold as MANY HYDROQUINONE CRYSTALS will filter out clogging up
the funnel. (then wash with DCM) or whatever.
28) Stopping Point -> once the ketone workup is started, don't stop until ketone is distilled then
seal it and put it in the freezer. Otherwise, ketone will be lost to temperature degredation.
29) When washing with NaOH...it must be cool to chilled as adding luke warm NaOH to DCM
boils the DCM (bp ~45C)...not good
30) When doing all the washes, keep a look out for solution temps. and don't put anything into
a solution of DCM that is warmer than luke-cool.
31) With a bit of swirling, emulstions between layers in a separatory funnel dissolve after 15-20
minutes or so. Or can stir with an extended coat hanger or shake with a vibrator.
32) When distilling ketone, use amount of buffer oil 50% w/w of safrol begun in the reaction.
33) Filter post reaction of hydroqyuinone through 3 coffee filters not just once, but do it 2 times.
Washing last of ketone through filter both times with eatra MeOH.
34) Take note of the temperature safrole comes over when distilling sassafras oil the first time
under vacuum. Whatever comes over at this temperature when distilling ketone is probably
safrole...collect it and disregard it...or reuse it...just don't send it on through to the MM al-hg
along with the good ketone.
35) Ketone and toluene form an azeotrope...so if distilling ketone don't do it in toluene
36) As per spric
a) Prestir 2g PdCl2 overnight with 400ml MeOH
b) Then add h2o and p-benzoquinone
c) Then continue stirring the mixture for 6 hours through the morning
d) Then add 180ml safrole slowly over 30 mins
- It heats up on its own to 60 c - then from the plate add more heat and within
15 min it should be 70-73c
e) Put the condensor on and medium stir for 3 hours results in 130g ketone on average
37) During the NaOH washes, if an emulsion forms it is possible to add more NaOH solution.
Making the solution more BASIC helps to knock out any emulsions that might form during
the NaOH washes. But before more NaOH solution is added, something to try would be
to add more DCM solution to the separatory funnel in an attempt to 'overwhelm' the
emulsion.
38) Also to see separations in the sep funnel...(NEW ADVICE HERE)...use a flashlight IN
TOTAL DARKNESS in order to see the separation of the two layers. Also, one might use
20% NaOH as the wash solution (instead of the 5% mm recommends) to make the soln.
in the separatory funnel more basic making separation easier and emulsions less likely.
39) DON'T FORGET WHAT MM SAYS ABOUT FILTERING OFF HYDROQUINONE AND PDCL2
BEFORE THE NAOH WASHES
"FILTER your solution thoroughly after the reaction and BEFORE the acid water flood!
This REMOVES the hydroquinone and PdCl2 that make the solution black (and
IMPOSSIBLE to separate during acid/base washes) if you don't. IF you do this
filtration, I GUARANTEE you that the separation during the first 5% NaOH wash (yea
that's 5%, not 10%) will be EASY as PIE, no problems WHATSOEVER seeing the two
distinct layers."
40) Antibody2: "after the normal post benzo washes, the dcm layer is more of an earthy dirty
kind of color, after the dcm comes off, you again have black syrup, which must be distilled."
41) - Two types of p-benzoquinone at photo shops:
1) green / yellow stuff (powder) - fresh and potent as a reactant
2) red / brown stuff (powder) - old and oxidized and bad to use this as a reactant
42) - Methyl Man says he uses the red / brown stuff in his benzo wackers. Other advice says the
red / brown stuff is an old oxidized version of the newer green / yellow p-benzoquinone.
Also, it might be good to prestir the red / brown p-benzoquinone longer than one would
prestir the green / yellow p-benzoquinone as the red-brown benzo is "chunkier / not as
powder-like" and might take longer to solvate into solution.
43) - MaDMax: - says he always used to get yellow / green ketone until getting a vacuum source
that pulled ketone over at 115 C.
- also says ketone gives menthol smell - kind of like a minty pine tree
- also says he gets tons of crap during the washings "you just need to
give it plenty of time and swirl it a bit to help all of the DCM make its way through the crap
layer and down to the bottom. (might be a good place to use the vibrator on the sep
funnel)
44) - MaDMax: - ALSO! ... : to further heighten yield...
Save all of the washes in a clean container. Any DCM that may have stayed in the wash
water layer falls to the bottom of the container. Just before one starts the NaOH washes,
one can decant h2o off the washes previously set aside and retrieve the extra settled DCM.
MaDMax suggests that one retrieves the DCM and puts it into the rest of the DCM before
the NaOH washes because these washes are pretty important for all the DCM to go
through. This process retrieves ketone that would have otherwise
been washed away.
45) - Methyl Man - says his ketone's aroma is like lime Kool-Aid with an artificial citrus-ish tangy
aspect that goes with the yellow-green color.
46) - Antibody2 - passes post benzo reaction directly through 1 inch of silica sand before doing
anything else. When this is done, 0 (ZERO) precipitation is created when hit with the 3N
HCl. He suggests also cooling post benzo reaction before filtering (in fridge for 1/2 hour)
so even more precip will be filtered out.
47) - HOT TIP: Hexane can be used to extract the tarry stuff left after the ketone distillation of
remaining undistilled ketone.
48) - Blue_Diamond says - the precipitate which forms after hitting with the 3N HCl is a
motherfucker and will clog up the separatory funnel. He doesn't prefilter his post benzo
reaction before hitting it with 3N HCl solution.
49) - If one begins the benzo wacker reaction with less than 178g safrole, just adjust the other
ingredients downward while keeping the reaction times the same.
50) - If one wants to 2x or 4x the benzo reaction, Osmium says multiply all chems by the same
amount but keep the reaction times the same.
51) - No matter what ANYBODY says, prestir everything in this reaction for
a long time as others report good/higher yields when doing this...and it certainly couldn't
hurt anything...just make sure to keep container sealed tightly (air-tight) when the stirring /
solvating is being done.
52) - If a fridge compressor is used as the vacuum source for vacuum distillations, make sure to
blow a high speed fan at it to cool it down the whole time its working.
53) - NEVER GET KETONE TO OR ABOVE 180 C WHEN DISTILLING...IT WILL
CARBONIZE
54) Handling and Using p-benzoquinone :
a) Pee green stuff (yellow-green) like flour - wear goggles and ONLY open the container and
work with the quinone UNDER A FUME HOOD. THIS SHIT WILL BURN THE FUCK OUT
OF YOUR LUNGS.
b) Reddish-brown course type - this type requires a lot longer pre-stir time in benzo wacker
but still BURNS THE SHIT OUT OF YOUR LUNGS WHEN INHALED. Wear goggles and
only work with this stuff under a fume hood. Actually, this reddish-brown course type is
regular pee-green p-benzoquinone that has been left in the air to oxidize and is not as
an effective an oxidizer when compared to the fresh pee-green stuff...don't use this stuff
if this kind is what is given as 'fresh' p-benzoquinone
55) - "Benzoquinone" is a "redevelopment toner"
Pea-Green = GOOD
Brown-Red = BAD oxidezed pea-green quinone
56) - When distilling ketone, add pre-distilled saflower oil to buffer the ketone solution so it won't
polymerize in the ROUND bottom distillation flask. Pre-vacuum distill saflower oil (under
the same vacuum mmHg) to ~40-50 C higher than what safrole came over at. This is to
ensure nothing in saflower buffering agent doesn't distill over at the same C the ketone
comes over (usually ~25-40C higher than what safrole comes over at at the same vacuum)
57) - Pull the ROUND bottom flask (distillation flask) out of the oil bath pretty soon after all the
ketone is collected or it will eventually polymerize and carbonize in the distillation flask (if
left in the hot oil bath).
58) - When doing all washes / separations involving a solution of water (acidic or basic) and
DCM.
DCM ALWAYS = BOTTOM LAYER
H20 ALWAYS = TOP LAYER
59) - Also...100ml dh2o + 5g NaOH = 5% NaOH solution
60) - NEVER, EVER, EVER let the reaction continue under improper stirring. A GUARANTEED
decrease in yields will occur if this happens
61) When adding NaOH to the post reaction mix workup: adding the NaOH to the mixed
ketone solution causes it to heat up a bit...SOOOOO...make sure that the NaOH solution
temp is a little below room temperature before putting it in and that the condensor is placed
on top of the vesses just after / during (NaOH dropped through the condensor) the NaOH is
added...Methyl Man says about this step..."if basification is not done cautiously and slowly,
the goods may get all pouty and decide not to cooperate later during the crystalization."
SOOOOO....the lesson here is, again, to add the NaOH solution slowly.
62) P-BENZOQUINONE SHOULD BE STORED IN AN AIRTIGHT DRY CONTAINER WITH
SOME SORT OF HUMIDITY ABSORBING PACKET INSIDE THE CONTAINER WITH IT.
P-benzoquinone degrades 4-5 days after being exposed to the air...suprisingly though...
'spric' experienced sligtly higher yields in his benzo reaction using p-benzo that was slightly
decomposed...it had begun to get a brown tint to it.
63) Spric's advice on increasing his wacker ketone yields
A) ODB has been getting 40g ketone from 160g safrole using these steps:
- 300ml DMF and 2g PdCl2 added to a 2L RBF
- stir for 14 hrs.
- add to the flask 120g p-benzoquinone and 50ml dh2o
- let stir an additional 2 hrs
- in a separate beaker mix 160g safrole and 50ml DMF
- add this beaker's contents slowly over one hour to the flask
- set flask up to reflux for about 7 hrs.
- filter the rxn. mixture
- flood the rxn. mixture with 1.5L slightly acidic water (100ml 31.45% HCl in 1.4L dh2o)
- separate the layers in a sep. funnel and keep the bottom layer
- extract the top layer with 2x 100ml DCM
- pool all DCM portions and the bottom layer (?)
- wash the pooled extracts in 1L saturated Sodium bicarbonate solution
- wash the ketone/DCM layer with 2x 500ml saturated NaCLll (note: at this point the
mixture thickens up and is hard to separate the layers)
- wash the ketone / DCM layer with 2x 500ml of 5% NaOH
B) Spric suggests the following:
1 - stay away from DMF and use methanol instead
2 - throw in an extra quarter gram or so of PdCl2
3 - throw in an extra 10 ml dh2o
4 - use b/t 130-135g p-benzoquinone
5 - make sure to stirr your palladium until it actually completely goes into solution
(usually 4-5 hours is good enough)
6 - prestirring p-benzoquinone in palladium solution doesn't seem to effect anything
at all.
7 - after about 10 minutes into the addition of the safrolesomething, turn your hotplate
up to a point where the reaction will almost get violent, that is the methanol is
boiling pretty decently.
8 - right when this happens, turn your hotplate down to maintain 50-55C rxn. temp.
9 - from addition, run the thing 6-7 hours
10 - try skipping those NaCl washes to see what happens, these don't change the
yield, but don't make much difference when distilling either.
note: running like this spric never gets less than 140g yield of ketone...the wacker
seems to like excessive heat...just keep a tall condensor handy...the press
says best results are obtained when it boiled out of control like an amalgum !
64) Above in note #67, spric suggests that heating the benzo wacker early during the addition
to a low rumble might help to increase yields. Might want to experiement with heating the
benzo during the begtinning as spric suggests while also giving it a similar heating
somewhere in the middle of the 6-7 hour reflux to see if this further increases yield %.
65) After doing all the washes, save all the washes together and then dump a bit of DCM into
the mix..."you'll be surprised at all the extra ketone you discover"
66) Antibody2..."Another way around that nasty NaCl emulsion is to put 20mL 31%
HCl into the sep. funnel, that'll straighten things out in short order. You can actually watch
the emulsion be devoured by the HCl...probably the only smile you'll get before the work-up
is over"
67) RollWitMe says "Wash your DCM layer
2x with saturated sodium bicarbonate. I think we all know about this crap (looks like frog
eggs / gunk / green apple splatter etc.) that forms in the middle. Well it contains a lot of
product so make sure you keep it with the DCM washes." so do it. Also...save all your
washes to re-extract once in the end.
68) One hiver has stated that some photo shops sell sodium palladium chloride labeling it as
regular pure palladium chloride and make it a point not to tell their customers the truth.
Sodium palladium chloride does not work with the wacker so make sure its pure PdCl.
69) When adding contents initially in the benzo-wacker, when adding water, do it right after
the benzo has been added to help wrinse the funnel
70) When distilling ketone, you really need a kick ass vacuum source.
71) Baalchemist finds new way to insulate culumn when distilling ketone.
Baalchemist:
"I got some of that SS mesh sleving that they use to dress up automobile hoses in the
largest size available. Then rounded up one of those SS fabric heating elements used
to keep the pipes from freezing in the winter. I wrapped the element around the column
spiraling from end to end, and fastened with a couple pieces of metal tape. Then took the
other SS sleve material and covered the element and column with three layers. Those
were held in place with a couple of hose clamps. What's nice is that those elements don't
really get that hot, but its just right for vac. distilling. All of this can easily be removed from
the column for easy cleaning.
Later in the thread:
tecnetium:
"Swim found that when distilling ketone that towards the end of the run that most of the
ketone was condensing on the thermometer and on the sides of the still head and
dripping back down into the reaction flask rather than coming over into the condenser,
even though heaps of foil was used for insulation. The solution: Use a small foot heater
to blow hot air onto the still head while distilling - soon as swim figured this out and
implemented this idea, heaps of ketone came pouring over into the receiving flask.
72) noj suggests doing two more water washes when working up ketone than any other writeup
written on the proces have ever suggested...because more water washes allows for more
ketone to come over...rather than getting stuck in the hydroquinone that is stuck in the
condenser. noj also suggests freezing the ketone and contaminants before filtering or
washing...this seems to solidify any quinone and helps to keep it in the flask before
dumping into the acidic solution.
73) kapten writes of issues not addressed thoroughly enough in the write-ups...
1) must have GOOD vacuum source when distilling ketone !
2) must have the strongest stirring hot plate available when doing the al/hg
74) weasil states - "The wacker definatly works better when the methanol is properly refluxing,
and not just sweating."
END OF NOTE SECTION ON THE MM P-BENZO WACKER
We hold these truths to be self evident.
(Stranger)
08-22-01 20:37
No 206590
SECTION THREE - Methyl Man's Nitromethane Al-Hg Animation of MDP2P to MDMA
NOTE: Page down to note #24 to read up on Methyl Man's latest advice about how
quickly to make the addition for best yield %. And what to look for to know if addition
is going too quickly or too slowly. Further note...more work has been written of since this was
originally written (MM's version) on how baalchemist (and others) are doing 2x and 4x times
the amounts of reactants in larger flasks and doing the addition in as little as 15 minutes. This
makes the reaction run extremely hot (so adequate head space and condensor cooling is
required) and allows for much higher yields so that 1g ketone = ~1.1g salt.
Materials:
27.5 g Reynolds Wrap Heavy Duty Aluminum Foil
25.0 g MDP2P ketone
20 ml MeNO2 (Nitromethane) of 99%+ purity
750 ml MeOH + 50 ml more
400 mg HgCl2
2L 2 neck FLAT bottom 24/40 reaction flask
400 mm reflux condensor
250 or 500 ml addition or separatory funnel
262.5g NaOH (make soln. by adding solid NaOH to distilled H20 ice cubes (pre-weighted))
31.45% muriatic acid (HCl) for gassing
cooling setup: bucket, water pump, tubing, large bag of ice, tub o-ring clamps, salt
Method:
1) Cut 27.5g Reynolds Wrap Heavy Duty Aluminum Foil into 1" x .75" squares (1.5 - 2 hrs by
hand with scissors).
2) Fill coffee grinder loosely (2/3 full) and grind foil for ~10 seconds. Will take 4-5 loads to d
all the foil. When done correctly (don't stuff coffee grinder too much or grind for too long), the
foil should be "gnarled little nuggets about the size of long grain rice grains and should look
really tight and small." The smaller the better for efficient stirring.
3) Place 3" stirbar into 2L FLAT bottom flask and only stirplate
- add foil nuggets to flask then setup the rest of the glass
- if using 1 head 2 L Flat bottom, then glass = claisen adapter, addition funnel, reflux
condensor, and cooling apparatus.
4) Carefully add 750 ml MeOH first, then 400 mg HgCl2 second to a tightly sealable bottle.
Shake to dissolve then set aside.
5) Combine the 25 g MDP2P, 20 ml 99% MeNO2, and 50 ml MeOH in a beaker then add this
mixture into the addition funnel. Rinse beaker with a tiny bit of additional bit of MeOH to
get residual ketone and add this to the ketone / MeNO2 / MeOH solution already in the
addition funnel
6) Very slowly and carefully (gloves, glasses, long sleves) pour (using a large funnel) pour the
HgCl2 / MeOH solution from step 4 down the condensor. - wrinse condensor down into
reaction flask with some MeOH...not much though.
7) Turn the stirring on full blast for a 5 second burst to immediatly mix the solution and the foil.
Then give it 3 more 5 second full blast stirrs over the next 3 minutes (helps to facilitate
amalgamation of Hg onto the Aluminum).
8) After ~ 5 minutes or so, one would begin to see bubbles popping up on the surface of the
MeOH solution. First tiny champagne-like bubbles, then larger like ones seen in boiling
water. Around this same time that the appearance of the Aluminum will change from
shiny silver to starting to take on a dull gray look, accompanies by a gray cloudy look that
begins forming in the MeOH. This is the magic moment to begin dripping in the MDP2P /
MeNO2 / MeOH mixture from the addition funnel. Set a drip rate @ ~2 drops per second
and NO FASTER !!!!! The drip rate can be increased later to accelerate the reaction if so
desired.
9) Place ~ 3 pounds of ice into a bucket. When exothermic heat can be felt by feeling the
outside of the reaction flask, quickly add ~ 2.5 L h2o to the bucket and plug in the pump
to begin circulating ice cold water through the condensor. Can put salt into the ice water
mixture and this will allow the water flowing through the condensor to be colder.
10) While monitoring the growing intensity of the bubbling amalgamation, turn on/off the
stirring intermittently as done earlier. This is to ensure even distribution of the ketone /
nitromethane into the reaction flask but also because the amalgamation seems to gain
its vital momentum more effectively if given some significant blocks of time (meaning ~
30 seconds at a time) in between stirring bursts. When the reaction is clearly starting
to get vigorous and hot, crank the stirring to 10 and leave it on.
11) As the reaction progresses a few minutes post addition, the aluminum should be breaking
up fairly rapidly. This is good as long as the ketone / nitromethane mixture is dripping in at
a good rate of ~2 drops / second. Be careful with the addition rate at this point because a
rate of greater than 2 drops per second will cause the reaction to kick into unwanted over-
drive...not good. The reflux condensor should be unnerving vigorous as the amalgamation
really starts to pick up speed: with the MeOH dripping from the condensor really quickly.
This is good. At this point, sludge can be observed already starting to settle at the bottom
and forming a ring on the inside of the glass around the top surface of the spinning mess.
Consistency will get thicker by the minute. Add more ice to the cooling bucket as needed.
12) At this point, the reaction can be slowed or sped up by controlling the addition rate. If the
reaction is already barreling along then no increase in the addition rate is needed. The
concept is: the addition of the ketone / nitromethane mix should be paced neck-and-neck
with the breakdown of the foil as it amalgamates and gets turned into sludge. Adjust the
addition so that the 2 processes progress at the same rate. Might want to keep some type
of apparatus ready to cool the outside of the reaction flask if it looks like the reaction is
getting out of control and the reflux condensor won't be able to handle the escaping gasses.
Could be as simple as a high speed fan blowing on the reaction flask while simultaneously
slowing the addition rate...to as aggressive as some type of luke cool water bath to dip up
and around the bottom of the reaction flask.
13) Addition should take between 40-45 minutes in total and when finished the state of the
aluminum should be ~ 95% broken down. 45 minutes past initial addition, the reaction
should look like a really thick, steely-gray chowder with only minor silver slivers of
undissolved aluminum visible if any at all. Probably will need to add 20-30 ml MeOH at
this point (or even before) to help it keep stirring effectively. Preheat MeOH before adding
though so as not to slow down the reflux upon addition. Or, if reaction is going to rapidly,
adding room temperature MeOH would be a good way to quickly directly cool the reaction
mixture.
*NOTE: on color: 30 minutes post initial addition, the reaction takes on a color that is
"light steely gray with blue overtones." Light shade of gray akin to the color of common
gray sweat pants, with a slight suggestion of blue. This color indicates a good reaction
with properly prepared aluminum foil. Dark metallic gray with green overtones suggests
too thick aluminum foil and not enough HgCl2. Green color comes from unreacted
ketone.
*NOTE: Also, on the timing of the addition against the breakdown of the aluminum: There
is a definite spike curve to the amalgamation reaction which is easily observed by
watching the reflux rate. This build up to peak and subsequent slow down occurs over
approximatly 25 minutes or so -- very fast. So at only 20-25 minutes after the
amalgamation was first felt to be heating up, the reflux will have slowed to ~2 drops per
second after having reached a peak where the reflux was a stream re-entering the
reaction flask and not drops. At 1hr 15min after the addition was begun the reflux will
be a slow 1 drop per 2 seconds or so.
Finally, when...
a) the reflux has slowed to almost no reflux at all
b) if no small bubbles can be seen anymore when the stirring is stopped
and c) no "uneaten" aluminum is visible and the solution is a thick, uniform gray soup...
then the reaction is essentially finished.
* - It will reach this state ~ 1hr 45min to 2hours after the initial addition was begun
* - At this point, add a bit of external heat where the addition has finished and the reflux slows
down dramatically
* - Leave the reaction stirring for a total of 3 hours AFTER the addition of the ketone /
nitromethane solution IS COMPLETED.
- Total reaction time is ~3hrs 45 min.
13) Turn off the heat and allow everything to cool (reflux condensor still cooling) for ~ 30 min.
14) Make a solution of 35% NaOH by adding 750 ml dh2o and 262.5g NaOH. Let this
solution cool back down to room temperature.
15) In a separatory funnel no smaller than 2000ml, pour the cooled gray reaction mixture. Use
a magnet outside of the flask to keep the stir bar from falling into the sep funnel which
of course would break it. If the gray mixture is really thick, MeOH can be added in small
amounts to thin it to a pourable consistency. Wash the residue out of the reaction flask
with a few mls of MeOH and add to the separatory funnel also.
16) Slowly pour the 35% NaOH solution into the separatory funnel (glasses and gloves).
Basifying should be a gentle process so pour slowly. Solution in the funnel will warm a
bit as the last of the aluminum foil (if any) dissolves.
* - Swirl this solution in the separatory funnel a bit and give it ~ 10 minutes or so to return to a
temperature closer to ambient...
NOTE - MeAm will smell here. MeAm smell = successful reaction though.
17) When the mixture in the separatory funnel has cooled, extract it once with 400 ml toluene
followed by 100 ml toluene. Shake at least 3 minutes (long and hard) for these
extractions (while venting).
* - Toluene product layer will be on the top
* - Give layers at least 15 minutes to separate
* - Separation is complete when interface of small toluene bubbles finally resolves and a nice
clean line can be seen between the layers.
* - Finish off with a 3rd extraction of toluene using 50-60 mls
* - Keep in mind a vibrator can help during this separation and any done with these
procedures.
NOTE: (actually a whole couple of added steps): The combined toluene extracts will
inevitably contain a tiny bit of base / metal / garbage from the bottom layer.
To separate this shit out:
1) chill the entire solution inn the freezer for ~ 30 minutes
- when cold the garbage is a lot less mobile
2) decant the toluene / product layer being vigilent around the last 50 mls. or so.
18) Now drain the garbage layer out of the previously used separatory funnel and wash the
garbage residue out of the separatory funnel with water.
19) Wash the toluene / product 4 times (or more) in the separatory funnel with 400-500 ml
dh2o and a final time with 500 ml dh2o saturated NaCl solution to remove any traces of
solvated HgCl2.
20) Dry the toluene / product solution with 30 g of MgSO4 (epsom salts) in an acetone
cleaned heat dried bottle or flask for no less than 45 minutes to 1 hr. Shake a few to 5
times during this drying period lasting up to an hour.
21) Filter the solution of the MgSO4 and gas it with that good ol' HCl bubbler setup.
* - note: be smart and use just enough muriatic acid (HCl acid) (31% HCl) to just wet
the salt but definatly not enough to make any puddles
* - And...put a wad of drying agent in line somehow between the gas
reaction flask and the tube leading to the pippette end
Expected Yield: 20.0 - 21.5 raw product that recrystalizes to 17.0 - 18.0 g MDMA*HCL
END OF PROCEDURAL STEPS SECTION OF THE MM NITRO AL-HG
Short Note version of Al-Hg :
1) 3" stirbar + 27.5g Al foil nuggets -> into a 2L FLAT BOTTOM 24/40 flask
2) add first 750ml MeOH then 400mg HgCl2 shaken to dissolve in a sealed flask / container
3) 25g ketone + 20ml MeNO2 + 50ml MeOH -> into an addition funnel
4) SLOWLY pour 750ml MeOH + 400mg HgCl2 (dissolved) down the condensor to the 2L RB
flask previously loaded with stirbar and Al foil
5) after short bursts of intermittent stirring (5-7 mins. later), Al is amalgamated -> not begin the
addition of ketone + MeNO2 + MeOH mixture @ ~ 2-3 drops per second
6) Add the ketone solution as quickly as the condensor allows
7) Add up to 100ml preheated MeOH soln. to rxn. flask to facilitate stirring
8) when reflux slows, add mild heat and reflux for 3 MORE hours
9) after 3 hrs., stop heat then let soln. cool to room temperature
10) Transfer cooled rxn. mix -> 2000ml sep funnel and add SLOWLY cooled soln. of 35% NaOH
(750ml dh2o + 262.5g NaOH)
11) Swirl well and let cool back to room temperature
12) Extract with TOLUENE 3x using 400ml, 100ml, then 100ml
13) Cool sealed and combined toluene extracts in freezer - then decant toluene from slower
residual trash layer - add 100ml more toluene to trash - rechill - re-decant - then combine.
14) Wash toluene / product 4x with 400-500ml dh2o
15) Wash toluene / product 1x with 500ml saturated solution of NaCl in dh2o
16) Dry toluene / product with 30g MgSO4 - filter then seal tightly
17) Now gas this solution directly with anhydrous HCl gas for xtalization
We hold these truths to be self evident.
(Stranger)
08-22-01 20:43
No 206591
NOTES ON THE AL-HG REACTION:
1) If using a round bottom flask for this reaction, a water bath can be used to heat the reaction
flask. Flat bottom works better though as it gives a good platform for the stirbar to spin on. If
using a round bottom flask make sure to use an egg shapped stir bar and not the long rod-
type stir bar.
2) Make sure to add more MeOH through whichever neck if the reaction begins to get thick and
doesn't stir as well. Also, the flask may be picked up and stirred by hand occasionally if this
helps to get the mag stir bar going.
3) If reflux starts to get out of hand, slow down the addition rate of the ketone / nitromethane
solution.
4) Add as much MeOH as it takes to keep the aluminum covered during the addition cycle...
Much MeOH is lost due to evaporation even with the condensor circulating ice cold h2o.
5) When the addition is done, try to break up the aluminum as much as possible (by hand
swirling?)
6) Cool the condensor to ice cold before the addition is begun to ensure higher reaction yields.
7) One states he adds up to 100ml MeOH after the addition to ensure the aluminum doesn't
sludge things up too much and the reaction keeps stirring well.
8) During extractions, shake as long as you can for as long as you can.
9) Blue_Diamond says - best runs were seen when the addition was fairly fast and the reaction
ran at a hot reaction temperature.
10) The reaction is refluxing too quickly when bubbles can be seen forming and rising inside
the condensor.
11) When washing the toluene / product layer with 4 or more water washes, if the 4th water
wash isn't clear, keep doing water washes until h20 is CLEAR. Have to let the h2o layer
sit a while to let bubbles get out which make it look cloudy. Water should be as clear
(after last wash) as it was before being put into the separatory funnel.
12) Methyl Man says - to add incrimentally enough MeOH during the reaction so as to keep
it stirring well at all times.
13) Methyl Man says - "you HAVE to make that puppy run HOT"
14) Get a high output water pump for condensor water circulation here to cool this hot reaction
down sufficiently. "Reaction should be really humming when you've dropped in 20% of the
nitromethane / ketone / MeOH mixture. Flask too hot to touch for 1/2 second. Should still
be this hot when the last of the nitromethane / ketone / MeOH is dropped in.
15) Bizwax says - it wouldn't hurt to let the reaction run 6-8 hours to make sure it is completely
done.
16) Water IS needed in this reaction so do not dry MeOH before using.
17) Coffee grinder = Black & Decker "Coffee Mill" (cat # CBM-1 Type2)
18) Stirbar = 3" egg / teflon coated
19) Use at least a 150 gph water pump for condensor water
20) The condensor water should always be super cold
21) Methyl Man says - "watch the vortex, if no vortex is noted then add incrimentally up to
~ 100 ml MeOH to help stirring commence again."
22) Methyl Man says - use a 400 mm Allihn for reflux for this reaction.
23) High-oleic safflower smokes when heated to a high C the second time, but its ok to use
the first time.
24) Methyl Man's latest advice on running this reaction (as of aug 6 '00):
- add the ketone fast right from the start 2 drops a second
- make sure the whole addition takes only 30 minutes...no more
- this gets the reaction DAMN hot
- reflux should be dripping so fast its almost POURING down
- use a 2L flask...NOT a 1L
25) To avoid MeAm smell during the reaction, run a tube or hose from the top of the condensor
to a 3 N solution of HCl. This will turn any gaseous MeAm into its HCl salt and eliminate
any aroma
26) When adding extra MeOH to help keep the reaction stirring, make sure to pre-heat the
MeOH to ~ 55-60 C before introducing to the reaction flask so as not to cool the
reaction contents too much.
27) Osmium says the al-hg works much better with 40% aquous MeNH2 as opposed to Methyl
Man's nitromethane version.
28) If using a fridge compressor / pump for the vacuum source, always cool it while in use
with a high speed fan blowing directly on it
29) Osmium says all the aluminum sludge must be removed before the ketone workup
(a/b washes / extractions) is done. If ANY aluminum sludge is left over it will TOTALLY
fuck up the a/b washes. If not sure that ALL the sludge is removed, then filter until
ALL THE ALUMINUM SLUDGE IS REMOVED WITHOUT QUESTION
30) MM says - the main things are
a) use Reynolds Wrap Heavy Duty Foil (THIS AND ONLY THIS EXACT BRAND)
b) use between 400 and 420 mg Hg salt
c) react the motherfucker DAMN HOT
d) make sure and keep the thing stirring the whole time...even if it takes adding MeOH.
e) after only 20% is added to the rxn. container, it should really be going HOT...flask too
hot to touch for even 1/2 a second and the condensor working furiously mad.
And it should still be that hot when the last of the goodies are dropped in.
continuing...about 5 minutes after the last drops have been added from the addition funnel,
the reaction should start cooling down...and at this point mm likes to start adding a bit of
heat to help break down the remaining aluminum
31) NEVER, EVER, EVER allow too much solvent (MeOH) to evaporate without adding more
during this reaction so that improper stirring ever occurs. A guaranteed DECREASE in
yield will result if PROPER STIRRING is not MAINTAINED at ALL TIMES .
32) Keeping enough methanol in the reaction mixture to ensure PROPER STIRRING is a big
determining factor in keeping yield % high.
33) Add 2-3ml dh2o to rxn. flask solution after the aluminum has initially amalgamated.
34)
a) Don't overgrind your foil in the coffee grinder - only a few seconds of grinding will do.
b) Be sure to use a big ass stir bar - violent stirring will up your yields.
c) Let your NaOH solution cool to room temperature before using ( DCM boils at just
above RT ).
d) Also...let your aluminum react completely (dissolve?) after your ketone addition...it may
even take over three hours.
e) Also...afterwards don't skimp on washing the toluene / product layer with water. Extra
washes help remove any remaining mercury.
35) Baalchemist ran mm al-hg with...
a) 31g ketone
b) 25ml nitromethane
c) 50ml methanol
- all the above well mixed in an addition funnel
d) 750ml methanol
e) 400mg HgCl2
f) 33g foil
- all the above in a 2 L reaction flask
* - addition done at 2.5 - 3.0 drops / second. Addition is finished in ~ 20 minutes.
* - addition was finished while rxn. was still in strong reflux
* - refluxed for 3.5 hours when reflux began to slow down a bit
* - workup (washes / extractions) were done as usual with a little extra toluene
* - epsom salts were added to the toluene to dry...stirred for only 2 minutes.
* - toluene soln. then hcl gassed to produce 31g product
* - the reaction runs REALLY HOT at this addition rate but if done in a 2L flask
it has plenty of room to spare during the hottest part of the reaction.
36) Baalchemist and
others have done some great work and have reported in this file upping the starting
reagents and adding them quickly to get a 1g ketone = 1g product yield %. Other tips
included in this file include adding 1/3 of total nitromethane to be used to the rxn. flask
directly after amalgamation occurs but before addition of the ketone / nitro / methanol
from the addition flask. Others = adding a small bit of h20 (2-3ml) to the reaction during /
before the addition and another is to reflux post addition completion for 4 hrs. or so. Make
sure to reread this file and ask questions.
37) Oct 3. - baalchemist says - preloading with nitromethane (1/3) gains nothing in yields in
quantities up to 50g. Frost agrees with baalchemist in this point and adds..."if no external
heat is available, and only stirring is available, it will help to break down the aluminum
better by adding 1/3 nitromethane first...which in turn will make for a better yield %...but this
is ONLY if no external heat source is available to aid the reaction post addition peak temp."
Bizwax agrees with baalchemist and frost on all these points
38) Reply to a pm to baalchemist - he says he gets better yield in the mm al-hg by speeding up
the addition rate. He says that mm has said (of his own original tek) that with the slower
addition of the ketone / nitromethane / methanol mix (30-45 min) that the aluminum foil is
too far broken down by the end of the addition...thus resulting in less product yield %.
Baalchemist says he increased the size of the rxn. a little and increased the addition rate
and now gets 31g salt from 31g ketone. Says he always worried about the volcano factor
during this reaction, but has found that as long as the condensor is super cold and if one is
is using a rxn. flask with plenty of headroom that faster addition can be accomplished with
no worries.
39) In a reply to a pm , baalchemist says - "been getting 32g salt from 31g ketone like
clockwork lately. I use 31g ketone, 26 ml nitro, 50ml MeOH - well mixed, added to
925ml MeOH, 125mg HgCl2, 37g foil. 3 drops a second addition rate usually does it.
Sometimes an additional 20-40 (or a little more) of MeOH is added to help stirring.
40) Baalchemists modified Al - Hg -
thread titled = "Baalchemist's modified Al/Hg"
- 36g Reynolds Heavy Duty in 1" squares ground for ~12 seconds
- placed in 2L flat bottom with magnetic stirbar
- add 100-120mg HgCl2 to 950ml (or a little more) MeOH, shake ~30 seconds, set aside.
- 31g ketone, 26.5ml nitromethane, 50ml MeOH placed in an addition funnel and mixed well
- add the HgCl2 / MeOH to the 2L with the foil and stir on 10 for 5 minutes
- attatch condensor and addition funnel
- then add 5lbs ice to the condensor circulation water
- after 5 min. stirring, turn stirrer off to check for bubbles coming up to surface
- if you see just fizzing, stir again for 3 min. then check for bubbles again
- If bubbles (not fizzing) are present, turn stirrer on 10 then begin the addition
- drip rate of 2.5 - 3.0 drops per second. (the faster the better here)
- might add an additional 75ml MeOH during the reaction to keep it stirring effectively
- addition should be complete in about 15 mins. foil is 1/3 - 1/2 broken down
- contents are grey with a noticeable blue hue to it
- when reaction reflux slows, add enough heat to keep it at reflux for 3.5 hours after the
addition and no more ("no more" time or "no more" heat ?).
- keep it stirring while cooling, then add 400ml toluene, then slowly add base solution
(300g NaOH in 825ml H2O).
- stir this for 30 minutes
- remove toluene
- add another 200ml toluene
- stir for 20 minutes, remove toluene
- extract with prolonged stirring with a last aloquat of 100 ml toluene
- combine toluene extracts and dump in 35g dried Epsom Salts
- stir for 1 min. - then let sit for 2 minutes
- then gas for 31-33g yield
- faster addition + less HgCl2 = higher yields
- also make sure you have a damn efficient condensor
- put a wad of paper towel in the top of your condensor to keep hold of stray vapors
41) Baalchemist's AL/HG twist = thread name
- 55g foil nuggets 50/50 mix of 1" square and 2" square
- in a 2L flask a 50/50 mix of 99% IPA, and MeOH were placed along with foil
- after making sure this vol of liquid would stir, 120mg HgCl2 was added
- stirring, amalgamation occurs and a condensor is fitted to the top of this amalgamation
apparatus
- 50g ketone, 40ml nitromethane, 50ml MeOH
- after 7 minutes, amalgamation was apparent and addition was begun at 3 drops per sec.
- addition was complete in ~15+ mins. and addition heat was added to reflux for 3 hours after
reaction begins to slow.
- stop, let cool, then transfer to a 3L beaker for basificaiton.
- 825ml H2O and 300g NaOH was then prepared
- 500ml toluene was added to beaker with stirring, the base solution was added slowly.
- stir 30 minutes then remove toluene
- do again with 200ml toluene
- do again with 100ml toluene
- combined toluene extracts were washed with H2O 3X
- then toluene extracts were washed with a saturated brine solution (NaCl water?)
- this was gassed for a total of 52.5g salt
- Methyl Man's comments on the above reaction after doing it himself..."did your ratios
and found the amount of NaOH you use is NOT enough to dissolve the aluminum. It
made for a sticky ugly dirty extraction process. 300g NaOH in 825ml H2O is just not
enough. I'd suggest doubling the amount used in the MM write up which would be
1500mL of 35% NaOH or something close to that. Also, I was timid running the addition
that fast and would feel much more comfortable running it in a 3L or 4L flask."
Baalchemist says - he "carefully pours nitro, MeOH, then ketone into addition funnel when
making the mixture." these layers of chems sometimes separate so this may be a fairly
important step he's mentioning here.
42) Make sure that the NaOH is a little below room temperature before putting it in and that a
condensor is placed on top of the vessel just after the NaOH solution is added. Methyl Man
says about this step..."if basification is not done cautiously and slowly, the goods may get
all pouty and decide not to cooperate later during crystalization." SOOOOO the lesson
here is, again, to ad the NaOH solution slowly.
43) When doing the Al-Hg addition step, have a high speed fan pointing at setup at all times.
This is to be used if rxn. starts to get out of hand and needs to be cooled quickly. If fan is
used a wet paper towell or piece of cloth should be placed over the condensor so the air
current won't blow any uncondensed vapors out of the condensor. Make sure rxn. setup
is well braced though so as not to be blown over.
44) MM says "at the 55g aluminum scale, the al-hg reaction, one 400mm Allihn reflux
condensor ISN'T enough."
45) MM conjecturing on the nature of the al-hg reaction while ultimate rxn. conditions are still
being researched (November 16, 2000)
"One key factor - and Baal and I are in agreement on this - is that there is a 'spike' in the
middle of the amalgamation process ... a place where it gets hottest based on how fast
the ketone had been added up to that point. Assuming a decent rate of addition in the
beginning, like around 2 drops per second, with experience one can take the reaction to
the brink of volcano-ness --- the spike --- and then stop the addition for a minute, let it
calm down, and then from that point forward it is less subject to go nuts and one can
speed up the addition significantly (with caution of course). Yields are ABSOLUTLY
LINKED to the rate the ketone goes in verses the rate of amalgamation. In other words,
if the aluminum looks mostly reacted, and you still have half your ketone in your addition
funnel, you will get a shitty yield. This is not news but it bears repeating because it makes
all the difference in the world ! "
46) When doing the addition part of the al-hg, make sure the glassware is setup so that the
heat / stirring source can be removed. This is so that if the reaction starts to erupt due
to the addition being done too quickly, the stir source can be removed out from under the
glassware (which stays suspended) and a pan of cold ice-water can be brought up
underneath the reaction flask to cool it off quickly. One of those platforms that crank up
and down would be an ideal platform to set the heat source on. This would allow the heat
plate / stirrer to be cranked down and removed quickly.
47) Baalchemist's entry on a hive al-hg thread:
"SWIM uses no more than 100mg of HgCl2 on reactions as high as 60 grams (al?) in a
2 L flask. SWIM cut the HgCl2 amount back because it slowed the reaction pace
(amal.) down and the intensity to a more workable pace, thus doing larger scale
reactions (60g) in that same 2L flask that was used for the 25g reactions. SWIM has
used as little as 40mg HgCl2 in a 60g reaction, but it takes much longer for the initial
amal. to kick in, but finishes like a champ with no probs. Definatly not one for the
newbees"
Take from this that maybe 100mg HgCl2 should be could be a good starting point
48) Nother exerpt from a al-hg thread from Baalchemist:
"Al foil (after being grinded in a coffee grinder) should not be too tight or it will adversely
affect reaction. This reaction's success depends on OPTIMAL stirring conditions.
49) Baalchemist's exerpt from an al-hg thread
"SWIM uses a lot less HgCl2 than MM, about 100mg. Try 2-3 drops in the beginning until
it refluxes hard and is about to blow, then
stop for a minute or so, then start addition again as fast as possible SWIM ran one the
other day with 30g+ ketone in, 34 out. That size reaction seems to produce the highest
yield % here.
50) RollWitMe writes of getting 22.5g product salt using ketone he usually gets 17-19g product
salt from by making a small variation in his usual al - hg reaction. He added .4g HgCl2 to
750 ml MeOH and stirred and heated it until it was boiling...then let it stand and cool to
around 55C. Added 27.5g aluminum and got what he describes as instant amalgamation.
He then immediatly began dripping in a mixture of 25g ketone / 20ml nitromethane /
50mL MeOH at a rate of 3-4 drops per minute. Workup was done the typical way, 35%
NaOH , extracted with toluene, washed 4x w dh20, 1x with saturated NaCL dh20.
Rotovaped down to 100ml, dried with 30g epsom salts...gassed, filtered, washed, dried.
He says he feels his extra product yield is due to adding ketone/meoh/nitro mix to an
'already pissed off' boiling amalgamation.
51) Stuffing coarse steel wool into a reflux condenser makes it work much more efficiently
during the initial addition and the subsequent refluxing that takes place in the al-hg rxn.
52) Tip from DiEthylEtherMan ... he does 3x al-hg with a 700mm with 15-18 minute addition rate
and his rxns. go 1/3 to 1/2 way up his condenser.
Tip: "after your 3 hour reflux with your al-hg ... let it cool but keep the stirring going. Turn
off heat 30-45 minutes before...after it cools remove the condensor and basify right
in the same container with the stirring still on high...this is how I've been doing it and
every piece of aluminum breaks down...the solution turns almost like a dark dark
blue / black color (thick) with no al floating around.
53) One bee writes of his theory that the al-hg reaches a bad spike in the middle when the
addition is done to a RT aluminum suspension because starting out cold
the ketone doesn't react well only slowly building heat as the addition continues. When it
eventually gets hot enough, all that unreacted ketone starts to react and then things really
get out of hand with bubbling through the condenser and shit. If the amalgamated
aluminum suspension is heated before the addition is started, the ketone being added
reacts immediatly and as it is added, thus, aleviating the risk that a ketone build-up will
occur which subsequently causes a large reaction temperature spike. Sounds good.
RollWitMe writes Feb. 19, 2001 - Add .4g HgCl2 to 750ml MeOH. Stirred and heated until
boiling. Let cool to ~ 55C. Added 27.5g balled aluminum foil. Basically instant
amalgamation. RWM knows that because the aluminum is floating on top and the solution
starts to turn grey. Immediatly started droping Ketone / Nitromethane / MeOH (25g / 20ml
/ 50ml) at a rate of 3-4 drops per second. A rxn. that he gets typically 17-19 g from he got
22.5 g salt.
54) Idea on how to cut foil strips:
Use a ruler or other straight edge on top of the foil leaving an inch exposed. Pull the foil
starting from the corner furthest from you and pull against the straightedge. You'll tear a
perfectly straight strip (well, mostly after you get the hang of it) . This cuts the foil prep
time down by at least 70% and you don't have to fuck up a pair of scissors doing it.
Another idea is to use a long straight edge (long metal ruler) but use an exacto knife all
on top of glass to cut the strips...then put the strips together and use a pair of scissors
to cut them into 1" squares.
55) Yet another saying that for this reaction to work well...it must be stirred VERY well. This
gives rise for the need for a really strong stirrer / hotplate combo
56) Some of the large use a paper shreader to create their foil strips first then cut
again, then grind the foil sheets till they are the size of rice grains.
57) Red water after the al-hg reaction is a sign that the ketone used in the rxn. was dirty.
58) terbium has said that a Friedrich condenser is more effective at holding back a strong
reflux than a Liebig or Allihn condenser.
59) Baalchemist says to use a 2.5 inch egg shapped stir bar with the al/hg. One must shave
the ridges near the center a little at a time until it fits through the 24/40 glassware joint.
Baal also says that hex shapped stir bars suck in sludgy environments.
60) terbuim has stated that a Friedrich condensor is much better at holding back a strong reflux
than a Leibig or Allihn condenser. A Friedrich condensor, though, should NOT be used in
a vacuum distillation setup
61) DiethylEtherMan...states that in the al/hg, it is ok to use only 200 mg HgCl2 as opposed
to using the 400 mg HgCl2 most write-ups suggest.
62) DiethylEtherMan...states that Toluene is getting harder and harder to get these days and
a great substitute would be Xylene. Just make sure to chill it before any gassing is done.
The only drawback he states is that uxing Xylene makes it take longer for the crystals to dry
completely but that this really isn't a problem.
63) Chromic states that a 400mm Allihn is the appropriate condenser for the al-hg...that a
250mm Liebig just won't do it.
64) noj says that stuffing steel wool in a condenser DEFINATLY helps to contain a reflux.
END OF NOTE SECTION FOR THE MM NITROMETHANE AL-HG
We hold these truths to be self evident.
(Stranger)
08-22-01 20:48
No 206592
SECTION FOUR - HCl Gas Crystalization
Chems:
- Non-iodized NaCl (table salt)
- HCl acid (muriatic acid at pool stores is 31.45%)
- Concentrated H2SO4 sulfuric acid must be at least 93% but 98% is much better
(if h2so4 is less than fuming, heat it until all water steams off and acid begins to fume...
then and only then is it conc. fuming sulfuric acid)
- drying agent to bubble gas through (MgSO4 or preferrably conc. fuming sulfuric acid h2so4)
Equipment:
- small separatory funnel / addition funnel
- side arm Erlemeyer flask (makes airtight junction with sep / addition funnel)
- aquarium tubing
- 12" long glass tube to be placed @ end of aquarium tubing
- drying agent in-line before glass tube and drying agent holding apparatus
-
- suck back container to contain any product liquid which might get sucked back into the
aquarium tubing if HCl gas slows and a neg. pressure is created in the system.
Method:
-1) Might want to use rock salt instead of non-iodized table salt.
0) Heat H2SO4 to drive off all h2o to fuming before using it.
1) Do ALL of this reaction outside as HCL gas causes EVERYTHING to rust or at the VERY
LEAST, for health reasons, do it all under a fume hood that will carry ANY AND ALL excess
HCL gas fumes away
2) Layer salt ~1-2 inches in flask
3) Make sure to place cover (with inlet hole for glass tube) over container to be gassed to help
reduce the amount of atmospheric humidity entering the dried solution
4) Barely dampen NaCl with muriatic acid - just make sure all salt grains are wet...no more
5) Slowly drip sulfuric acid in from addition funnel above
(that's about it)
How to know when to stop gassing:
a) stop gassing when pH is between 5 and 7
b) filter off crystals which will make the pH rise again
c) re-gas until pH again decreases to between 5 and 7
d) Colour change is a sign of over gassing when your toulene goes from yellow to red.
NOTES ON HCL GASSING FOR CRYSTALLIZATION:
0) MUST MAKE SURE THE SOLUTION ONE IS GASSING IS ABSOLUTLY DRY BEFORE
ATTEMPTING TO GAS. IF THE SOLN. IS NOT DRY THEN ALL SALT WILL FALL OUT IN
THE FORM OF AN OIL AND NOTHING WILL PRECIPITATE...MUCH WILL BE LOST
1) Make sure the container one is gassing into has a large opening as the salted out product
must be scraped out by hand.
2) ALL SOLUTIONS MUST BE DRY (including the toluene the product is in and the HCL gas).
3) Make sure salt used is baked and dried before using
4) No puddles should ever be present in NaCl layer...no puddles of HCL especially and also no
puddles of the h2so4 being dripped in.
5) Epsom salts can be cooked @ 550F for hours and still not be dry. But then it'll be rock
fucking solid. Find a medium where (highest temp.) the salts can be baked for ~ 2 hours
and not be rock solid and still be usable.
6) Make sure to put an empty wash bottle in-line just before glass tube to save product if
suckback occurs
7) To dry gas, one must bubble HCl (g) through concentrated h2so4 to do it effectively.
8) Suckback is caused by too slow a drip rate of h2so4 into NaCl dampened with HCl.
9) NEVER GAS IN DCM...ONLY TOLUENE
10) Yellow droplets collecting on inside of gassed vessel indicates non-anhydrous conditions -
probably coming from HCl...bubble HCl through concentrated H2SO4 before it hits the
toluene / product layer.
11) Have a beaker / glass full of water standing by (saturated with baking soda) when HCl
gassing to receive the remnants of reactant gas (HCl) when xtalizing is finished.
12) When gassing procedure is done and all the white is filtered out...tightly (air-tight) cap the
remaining solution and put in the freezer overnight to cool the solution. This will give some
more hcl crystals after the solution has cooled down for a while.
13) Might want to wash filter cake (MDMA*HCl) with freezer cold ANHYDROUS acetone to
remove more discoloring impurities. Shoud lose ~ 10% weight doing this step.
14) Acetonitrile - is a great solvent for crystalization if you can get it. Might be good for later
on if can get this solvent. Note to do more research on this solvent later on.
15) HCl gas EATS THROUGH VINYL hose (the clear stuff at Home Depot), but DOES NOT eat
through RUBBER hoses. Sooo...use rubber hoses to pipe HCl gas with instead of vinyl
hoses.
16) Felix says - add the H2SO4 SLOWLY
17) Bizwax says - When gassing - only put enough HCl acid in salt so that all the salt is wet /
not dry, and NO MORE....DEFINATLY NO PUDDLES
18) One poster says he stirrs freebase / toluene solution FULL SPEED when gasing with
glass HCL (g) tube 2 cm below the surface of the stirring solution.
19) When gassing, when HCl flow slows down enough (from the end of the pipette) so that the
end of the gass tube begins to get clogged with *HCl salt, remove the tube from the toluene
/ product liquid layer until HCl (g) production rate increases. When gas slows and salt
forms in the glass tubing, this means suckback is just around the corner so remove the tube
from the product to reduce the chance of this happening
20) Also, same file as #20 above, if / when any h2so4 'puddles' form in the salt layer when
dripping h2so4 onto mixture of hcl (l) and NaCl (s) when gassing, it is ok / good to swirl
the beaker around a bit to redistribute the h2so4 puddle.
21) From improv_chem:...When gassing is complete and no more white stuff is forming, filter
out white stuff and add a little distilled water (~5ml per 100ml solvent) and shake the shit
out of it for a while until the solvent gets clearer. Then separate off the water and pour it
onto a plate on your hotplate on low with a fan blowing on it. When all the water has
evaporated, scrape off the remaining product. This helps when hcl gas crystalizing all
kinds of amines.
22) After gassing, ALWAYS put filtered gassed solution in the FREEZER OVERNIGHT and a
couple more grams will crash out.
23) MUST bake NaCl salt (table salt) to dry it before dampening it with HCl acid to be used for
creating HCl gas.
24) On gassing...this is what LadyEthyl has to say:
- "as long as your mixture, sulfuric + rock salt, doesn't get too hot, you won't have a problem
with your gas line spewing moisture...if this happens you're screwed. You can avoid this
by varying your gasline diameter and using longer lengths. If you see moisture start to
climb, back it off. Also, if your oil has water or other garbage in the bottom, separate that
stuff out before gassing...with it in there one is sure to have problems when gassing."
25) It DEFINATLY IS possible to overgas and bring the pH down too low. Because of this, do
one of two things...1) fractionally separate out salt product at different periods during the
gassing process to save what has already percipitated out...or...2) find a way to measure
the pH of the solution being gassed and check it every so often during the gassing
process.
26) If too much water is introduced during gassing, after / during hcl gassing a tiny water layer
will form in the beaker being gassed below the non-polar layer and a lot of product will be
solvated in that small layer of water.
27) Note: evidently HCl can be found in canisters and is used by electricians somehow or
another
28) When finished gassing (DONE OUTSIDE) stopper the rxn. vessel immediatly (the vessel
the gas was created in) and remove stopper only when whole apparatus is UNDER
WATER (possibly a bucket of water) ..
29) One guy has found that it is better to gas two container with 3-4" of liquid than one larger
container with 6-8" of liquid.
30) Probably need to distill store bought H2SO4 before using it to gas with as it probably isn't
CONCENTRATED Sulphuric Acid (93%). Heat it up until it smokes...this means that most
all the water has been dirven off.
31) Putting undried mdma.hcl crystals in a round bottom flask and evacuating the air with a
vacuum is a good way to speed up the drying process.
32) Chromic says that in crystalization and recrystalization, leaving the anhydrous solution in the
freezer for 2 hours is necessary to get all the crystals out. At room temperature, all the
mdma will not crystalize out no matter how much the conditions are anhydrous and no
matter how much gassing is done...2 hour trip to the freezer is definatly necessary.
END OF NOTE SECTION ON HCL GAS CRYSTALLIZATION
RECRYSTALIZATION AS PER RHODIUM:
1) Dissolve crystals in minimum amount of boiling IPA (isopropyl alcohol)
2) Let the solution cool to room temperature
3) Add dried acetone with stirring (@ room temperature) until mixture becomes cloudy
4) Cool in freezer (stoppered air tight) for 12 hours.
5) Filter
RECRYSTALIZATION AS PER METHYL MAN:
1) Dissolve crude product (20g) in 75 ml of well filtered boiling anhydrous IPA
2) When all in solution, slowly dribble in 300 ml well-filtered freezer chilled anhydrous
acetone
3) Seal airtight and put in freezer
4) Wait one hour then filter
Notes:
1) No matter how pure H2SO4 is before using it for crystalization, make sure to heat it up and
fume it (dry it) before using it.
2) Before gassing, make sure to dry NaCl salt in an oven before using it to make dry hcl (g).
END OF NOTE SECTION ON HCL CRYSTALIZATION
We hold these truths to be self evident.
(Stranger)
08-22-01 20:53
No 206593
SECTION FIVE - GENERAL NOTE SECTION ON ALL REACTIONS AND PROCESSES:
1) Fridge compressor vacuum pumps may give out prematurely. If using one cool it down with
an external high speed fan blowing on it.
2) Can use 2 head claisen to adapt both a condensor and an addition funnel onto a 1 headed
24/40 flat bottom flask in the Methyl Man al-hg instead of using a 2 head flat bottom flask
as Methyl Man suggests to.
3) Long rod stir bars do not work well in ROUND bottom flasks...egg shapped stir bars are
needed here.
4) Always use 2-3 wraps of teflon tape on all joints when vacuum distilling from top aspirator
threads (where it goes into the sink head) to hoses and nipples. For 24/40 joints use
Super Lube found at www.super-lube.com - comes in a silver blue tube...use a match
stick head sized bead for each connection...that's all.
5) Use plumber's insulation cut to size for insulation of distilling apparatus = Thick fiberglass
cloth.
6) Let post reaction cool in MeOH Methyl Man benzo wacker before filtering out hydroquinone.
This helps when filtering out the hydroquinone onto the filter paper.
7) Blue_Diamond says - his best runs with the Methyl Man nitro al-hg animation involved a
"fairly quick addition" of the ketone / nitro into the solution / reaction and these reactions
had a really hot reaction temperature.
8) An indication the al-hg is going too vigorously is when water bubbles in the condensor and
is pushed upward / cracking / falling back into the solution by rising vapors in the condensor.
9) When the Methyl Man al-hg reaction becomes thick - like oatmeal thick - additional
methanol was added (pre heated) to get things moving again.
10) Fluctuating water pressure will cause aspirator to vary in vacuum pressure which, in turn,
causes bumping in the reaction mixture - NO, causes not the bumping, just vary
11) When gassing - do not use a gas diffuser - use a length of glass tube on the end of some
aquarium tubing.
12) To ensure one doesn't over-gas:
1) gas toluene / product layer
2) remove crystals (by filtering; but better simply centrifuging the crystals to
bottom and regassing the now clear top toluene layer again)
3) continue gassing and removing crystals incrimentally until further gassing shows no
further crystal development
- filtering ensures that if the toluene is over acidified, the product crystals will have
been previously removed unharmed
13) The beaker (or whatever) full of H2SO4 (in-line drying agent) should be filled with shattered
small pieces of glass to force the HCl gas to run a gauntlet of interfaces before it exits
the container.
14) If all the Methyl Man nitromethane al-hg amination results in less than all the foil reacting
and poor crystalization follows, this may be a sign that the foil nuggets were ground
too tightly.
15) To make a water aspirator more quiet, wrap towels above and below it. A piece of latex
hose going down through the "S" trap below the sink drain helps to make it quiet and
helps to increase realized vacuum pressure also. NOTE: If using aspirator, run it from
the main water line ... this should increase h2o pressure (and vacuum pressure)
significantly.
16) Sodium Cyanoborohydride gives 80-90 g MDMA-HCl per 90g ketone. Very scalable
also. Only need GOOD MeAm and this process is killer.
17) Don't fuck up with connecting water hoses to the condensors. Make sure to use hose
o-ring clamps (or nylon wraps,) so water don't end up spraying everywhere,
fucking shit up
18) To avoid the smell of MeAm during the MM al-hg, one can lead a tube from the top of the
condensor to a glass of 3N HCl to turn MeAm (gas) into its HCl salt.
19) Osmium says using 40%% aq MeAm in the Al-Hg works well.
20) Osmium says Methyl Man's Benzo Wacker can be 2x or 4x if all the reaction
chems are multiplied by the same number but the reaction times are kept the same.
21) Most organic solvents are heavier than water so putting them down the sink will get them
trapped in the PVC pipe's low spots eating a hole in the shit so don't do it.
22) Put salt into condensor cooling water bucket(along with ice and h2o of course) - the salt will
make the ice liquidize at a lower temperature, a coolant-coldermaker.
23) Also, keep recirculating condensor cooling water in a STYROFOAM COOLER to help it
stay cold ! Especially when doing ketone distillation and Al-Hg addition reactions.
24) WHEN DISTILLING KETONE...NEVER LET IT GET ABOVE 180C...IT WILL CARBONIZE
25) At least, if a fire extinguisher isn't readily available, have a wet towel always on stand-by
when reacting or distilling. And a box of baking soda. And bucket dry sand.
26) Good device to use when transferring / decanting liquids...30-50cc feeding syrings (found at
farm stores) coupled with clear vinyl aquarium tubing. Can use to suck up liquids very
accuratly. Never never use a turkey baister...they suck and don't hold liquid well.
27) To see how much vacuum an aspirator or pump pulls, boil water (at rt) with it fully pulled
down. See what temp the distilled water boils at...then go to Rhodium's site and look up
the vacuum / h2o boiling chart..."the very last article in the forum" (bottom of his page)
re: "vacuum pumps"
28) The more expensive metal water aspirators pull 40-50% more vacuum than their cheaper
plastic counterparts.
29) Make sure to get an aspirator that has a ball-type valve that doesn't allow suckback if
water is turned off.
30) Can reuse DCM (2-3x) a number of times if one takes the time to re-distill it between
reactions to purify it on its own.
31) The pro's use silicone oil for their hot oil baths
32) Of course, more smaller washes / extractions are better than a single wash / extraction
using the same volumes of solutes.
33) When using an aspirator, make sure to put a water trap in-line with the vacuum hose to
make sure the h20 doesn't suck back into distillation receiving flask if h2o is turned off
before the vacuum line is removed from the aspirator...ALWAYS REMOVE HOSE FROM
WATER FAUCET ASPIRATOR BEFORE TURNING OFF THE WATER TO PREVENT
SUCKBACK ONE WAY OR THE OTHER.
34) When washing final product crystals with acetone, make sure to DRY the acetone first or
crystals will disolve into the water still in the acetone. Also...make sure the acetone is
not only EXTREMELY DRY but also FREEZER COLD before using it to wash crystals.
35) To get rid of emulsions, one might run the whole mess through a buchner funnel to break
things up a bit. Afterwards let it sit a while to let the layers separate.
36) To avoid vacuum fluctuation when using a regular lab grade pump or even a fridge
compressor pump, make sure the pump is plugged into a different circiut than the
hot plate is plugged into. The hotplate kicking in is enough to disrupt the entire
circuit's entire voltage thus effecting the vacuum pump's efficiency. Also, make sure
there are no other "ON / OFF" type of circuit disruption occurring on the circuit the
vacuum pump is plugged into. Room heater, water heater, or whatever other household
appliance.
37) When makeing a solution of sodium hydroxide in water, first make distilled h2o ice cubes
(as many as possible) and add the solid NaOH directly to the ice (weigh the ice first of
course). This is because NaOH in H2O creats boiling heat and must be cooled down
before it is used as a wash solution...especially in DCM (bp 40 C).
38) ALL flasks being used in a vacuum distillation setup MUST be ROUND bottom and not
FLAT bottom. This includes BOTH the DISTILLATION flask AND the RECEIVING flask.
If EITHER of these two flasks (distillation OR receiving) are not ROUND bottom, either or
BOTH of them might implode.
39) Place vacuum gauge not in the main line but off the main line with a valve between the
vac gauge line and the main line. This is to keep the valuable vac. gauge away from
continuous vapor exposure which will degrade the gauge over time. Only open the stop
cock on the valve when a pressure reading is desired then close it to reisolate the gauge.
40) To dry acetone - bake MgSO4 - dump it in...stirr it...let it sit...filter off...good enough.
41) KEEP P-BENZOQUINONE OUT OF THE AIR - IN A DRY AIR-TIGHT CONTAINER
Drying packets should be in container with it. When exposed to air, it goes bad after 4-5
days. Funny thing is 'spric' got higher yields in his benzo with slightly decomposed
p-benzoquinone...it had started to get a brown tint to it.
42) ALWAYS CLAMP ADDITION FUNNELS...ESPECIALLY DURING ADDING H2SO4
TO MURIATIC SALT MIXTURE TO CREATE HCL GAS
43) Always pre-wet a filter with clean solvent before running anything through it to filter it of
a solid...pre-wetting the filter causes it to stick to the filter funnel (whatever kind
used)so that no solids get around the filter when solvent is first being poured on top of
it.
44) Make sure all glassware (24/40) is designed to accept some sort of metal clamp
at its joints to ensure glassware doesn't at any time fall apart, risking breakage, when
being used...Also...only use metal clamps (as opposed to plastic) as Osmium has said
the plastic ones are cheap and will melt and sometimes break
45) Make sure to use clamps on all glassware connections
46) Drying agents clump when they soak up water...so how much drying agent is
enough? There should be enough so its free-flowing in solution and not clumped up...then
you want some more in there too.
47) For cleaning glassware...a mixture of regular insoluable table salt in acetone makes a good
solution for cleaning the inside of glassware...the salt remains solid and makes for a good
abraisive element swirling inside the flask to clean it...and the acetone serves as a good
solvent.
48) Store ketone, always, purified or not, in the freezer in a light proof container...wrap foil
around the container, if needed, to keep light from getting in.
49) On drying solutions with MgSO4
- before dumping dehydrated MgSO4 into a solution to dry it, prewet the MgSO4 with
pre-dried solution so that it doesn't absorb much of it (along with product) when it
is dumped into solution
- after filtering dried solution of MgSO4, rinse the filtered MgSO4 with pre-dried solution
to remove any product that may be sticking to it.
50) Acetone + peroxide make a good glass cleaner...from sYnThOmAtic Do not heat the acetone
away, or explosions can occure!
51) When doing all vacuum pump distillations, even if joint grease is used, still wrap teflon tape
around the edges of all glass joints. From various posts, this does indeed make a
difference in the ultimate vacuum achieved.
52) One thing is to put a cut off valve inline between the pump and the distillation apparatus ...
close it before turning the pump off because sometimes when the pump is turned off some
vapors from the pump get pulled back into the distillation glassware and tend to add
unwanted junk to the distillate.
53) if using coffee filters as filters in a filter funnel, they should be UNBLEACHED
54) For a vacuum gauge it is suggested that one use a "mercury manometer gauge" rather than
a cheap round analog mechanical gague...the mercury manometer is much more
accurate. A good digital readout gauge is expensive, but good.
55) DiEthylEtherMan comments on what he's seen in his reactions when he unknowingly used
synthetic sassafras oil rather than the real thing. Synthetic sas = slow reflux during the
al-hg reaction and the safrole and ketone during these reactions don't burn when a small
bit of it is placed on your tongue. Real Deal Sassafras = vigorous almost uncontrollable
reflux when doing a 15-18 min addition during the al-hg and does sting a good bit when
both pure safrole and ketone (saf slightly more so than ketone) are placed a little bit on
your tongue. The end reaction is, after gassing, a very little bit of dirty tan / brown
crystals. Urban Legend class, never heard from synthetic sassafras
56) One bee suggests if having unexplainable problems in rxn yields to distill all your otc
solvents suggesting that otc chems are likely to be side products from industrial rxns. and
aren't always that pure to start with.
VERY good advice !!!! Do not stubbornly repeat the same faults, check the problem, one
by one, so begin with doubting your bought chemicals after more than 3 fuckups.
57) Have read advice that rotary vane pumps are better than diaphram vac pumps. NO!
58) All stopcocks must be greased or they will stick in their joint. A trick to get one unstuck
is to soak it completely in coke for 24 hours and this should help to get it unstuck.
59) ChemReack warns against getting a diaphram pump...says rotary vane pumps work much
better and then one could graduate up to compressors. Osmium says 'it depends on what you
want to do...a diaphram pump is more versatile.' and much better corrosion-resistant
60) One states that "Heet" gas line dryer may be contaminated with some sort
of rust inhibitor in it.
61) July 19, 2001 - Pugsly posted on hive about DEA possibly putting stuff in HEET and
ISOHEET to disable it as a solvent. As of Aug. 10, 2001...still don't know if its true.
Urban legendary BS. Just distill the shit then, so why does he think the DEA would
ever take it even in consideration?
62) GENERAL SAFETY NOTES AND NOTICES:
a) if an acid has splashed onto skin, fill sink with water, dump sodium bicarb (baking
soda) in sink full of water and dunk affected area in sink water.
b) if a base burn occurs, dump vinegar directly on skin
A) You better first wash with LOTS of tap water. If burn went unnoticed, then a)
and b) follow.
63) "Concentrated H2SO4 is like syrup." So if available H2SO4 is liquidy and not syrupy, then
carefully distill (heat it) until it fumes...then its concentrated. Might want to ask
though, on the net, if this is a safe procedure or just how exactly it should be done.
No Newbee should try it.
END OF ... GENERAL NOTE SECTION ON ALL REACTIONS AND PROCESSES
****************************************
PARTIAL EQUIPMENT LIST:
crankable platform (up and down)
2L ROUND BOTTOM reaction flask 24/40
glass thermometer
glass thermometer adapter
teflon tape
joint grease
hotplate / stirrer
teflon stir bar (3" long) and a second one possibly for stirring water baths
rigid glass tube for gassing
condensor - at least 40 cm -
vacuum adapter 24/40
synthetic tubing for water cooling
o-ring clamps, nylon straps, to secure tubing connections to glassware and other apparati
water circulation aquariumpump to circulate water through condensors
bucket to hold ice cold circulating water
claisen adapter 24/40
receiving flasks 24/40
metal clamps to hold glasware together
pH papers - full range
aluminum foil - Reynolds Wrap Heavy Duty
insulation for wrapping around distillation apparati
good milligram scale
mortar and pestle
2L separatory funnel 24/40
2L addition funnel 24/40
Buchner filter funnel 24/40
filter paper
coffee filters
Erlenmeyer thickwalled vacuum flask with side arm nipple
vibrator for aiding separations and emulsions in separatory funnel clear up
ventillation hood with spark proof fan
fire extinguisher
SAFETY GOGGLES ... SAFETY GOGGLES ... SAFETY GOGGLES !!!!!
good rubber or chem resistant apron
various other mixing / holding containers - flasks, beakers
graduated cylinder
coffee grinder to make aluminum foil balls
non-gas oven to dry MgSO4
suck back container, a.k.a. washbottle
some 24/40 glass stoppers or rubber stoppers
digital vacuum gauge or mercury manometer vacuum gauge
vacuum line thickwalled tubing
plumber's insulation
strong magnet - for retaining stirbars in containers when dumping out reaction contents
hygroscopic packets - put in p-benzoquinone after opening it up to keep it from oxidizing
oil for oil bath, peanut or silicone
lots of ice cube trays to freeze distilled water
CHEMS:
Methanol (MeOH) - Heet may have rust inhibitors in it ???
para-benzoquinone
MgSO4 - drying agent, only when pre-baked btw.
saffrole
distilled water
DCM - dichloro methane or methylene chloride
NaCl - non-iodized table salt
31.45% HCl acid - muriatic acid
concentrated H2SO4 - 99%
PdCl2 - palladium chloride or Palladium (II) Chloride - some photo shops sell it but it's really Sodium palladium chloride - not usable in the wacker oxidation.
NaOH - sodium hydroxide
Sodium Bicarbonate - baking soda
aluminum foil - Reynolds Wrap Heavy Duty
HgCl2 - Mercuric Chloride or Mercury (II) Chloride
Acetone
Toluene
Nitromethane
vinegar - to use in case of basic burns
sodium bicarbonate (baking soda) to be used in the event of an acid burn
We hold these truths to be self evident.
Edits in RED by LT/ + a lot of typo's corrected in this Section Five post.
(Stranger)
08-22-01 21:04
No 206596
There it is...turned out to be a lot longer than I first thought. If the mods think this would better belong in the newbee forum, please do move it over there. After posting this huge thing it appears as it might better serve as a fairly comprehensive methods write-up for those who haven't been gleaning the forums here for months on end.
a
We hold these truths to be self evident.
(Stranger)
08-29-01 04:55
No 208197
Also...Read Post 198797 (Dope_Amine: "MDMA the Phase Transfer Catalyst", Methods Discourse) & Post 199130 (Dope_Amine: "Re: MDMA the Phase Transfer Catalyst", Methods Discourse) given to us by Dope_Amine
We hold these truths to be self evident.
(Hive Addict)
08-30-01 02:01
No 208449
Didn't read much but it looks useful for newbee's.
Anyone attempting the Ozone generator bee careful, I have already read about one person burning their house down with such a setup!!! It will work however
Do Your Part To Win The War
(Stranger)
08-30-01 05:01
No 208486
No kidding foxy? I didn't know this type of device had that kind of potential or I would've given a word of warning along with the construction directions. Like I said before, I do know it'll shock the shit out of you if you contact even one side of the glass panel's sheet of wire. It is important though to separate it, insulate it from other objects. For mine I've built a cpvc framework to hold the glass pane relatively vertical. The cpvc doesn't touch any of the metal on the piece...only the 1" border of bare glass. I've been running mine continuously for about 4.5 months now and haven't noticed the first bit of heat generated. Again...it is well insulated.
Yea...the write-ups can generally be found anywhere here at the hive. And actually I could have left 'em out. Where people might find good info. for themselves is actually in the notes section following each of the rxn. procedural sections.
a
(Chief Bee)
08-30-01 13:54
No 208609
I generally don't like this writeup, as it has significant errors here and there. For example, the cleaning solution suggested (acetone + hydrogen peroxide) will create the powerful and unstable explosive acetone peroxide. Not a good thing. Another thing is that HCl gas will definitely corrode red rubber tubing, making it hard and brittle. White butyl rubber can withstand HCl gas however. That was just two errors I found skimming through one of the pars of the text. There are several very good tips in the text though, but a chem newbee cannot tell them apart from the ones that are potentially dangerous or completely unnecessary (like baking NaCl to "dry" it and then adding aqueous HCl).
(Stranger)
08-30-01 22:33
No 208736
Hey...whats up Rhod,
Oh man...my heart sank when I read you were disappointed with this file. I had hoped this would be a one-stop compilation of procedural tips for some of us more inexperienced reactioneers; instead it looks as if it might be more towards the 'Anarchists' Cookbook.' Please...do feel free to delete anything from this write-up you feel is un-noteworthy or unnecessary, and especially if it suggests doing anything dangerous like creating an explosive compound. Thank you, though, for pointing out at least these two pieces of misinformation. If I could still edit the original document I'd go ahead and take the time to eliminate those two issues out right now. But your mentioning them may be enough to swade future dreamers away from those two practices.
We hold these truths to be self evident...maybe
(Stranger)
08-30-01 22:50
No 208744
Well...because I've intended for this thing to be a one-stop, I'll copy and paste instead of just
giving the post #'s.
Post 198797 (Dope_Amine: "MDMA the Phase Transfer Catalyst", Methods Discourse) - Dope_Amine
MDMA the Phase Transfer Catalyst
mdma, mda, and 'tone are all phase transfer catalysts to varying degreese so for
my scrotum's sake USE BRINE DURING EXTRACTIONS. Otherwise, your yield might
take a bit poo poo (or you'll need to use way more solvent for the same effect.
Saving and stripping your junk layers is always a good idea too for those yield
obsessives out there (as if I need to tell ya this).
hibye...
Post 198978 (Dope_Amine: "Re: MDMA the Phase Transfer Catalyst", Methods Discourse) - Dope_Amine
Re: MDMA the Phase Transfer Catalyst
You're right zool, when you are separating dcm+goodies from an aqueous layer,
add brine and watch as more product and solvent falls outls out. I think this is a major
point that causes some people to have lower yields.
Anywayz zool, where's the gate keeper? Cuz I'm tha key master.....
Post 199130 (Dope_Amine: "Re: MDMA the Phase Transfer Catalyst", Methods Discourse) - Dope_Amine
Re: MDMA the Phase Transfer Catalyst
Oh, and with the stripping part, I was mainly referring to the solvent from which
ya crystallized.
Also when you separate the acid layer from the DCM layer, it is good to extract
that DCM layer with another bit of acid. This is again b/c of that PTC nature of
the product.
(Stranger)
10-06-01 06:26
No 220847
Acetone and Hydrogen Peroxide will usually not make
Acetone Peroxide unless it's in the presence of an acid.
I used to make Kilo batches of it and trust me it's _really_
easy to do. It's not explocive unless it gets cleaned up.
I couldnt get it to go off unless it was dry and the excess
of Hcl will try to inhibit the explocive of this Acetone
Peroxide. The REAL danger is the threading of jars... the
threading will dry out and leave a powder and the friction
of taking the lid off could make the explocive detonate.
Acetone Peroxide is a Primary Explocive
Gott Mit Uns!
(Hive Bee)
11-03-01 00:36
No 232296
"USE BRINE DURING EXTRACTIONS"
swim feels stupid asking, but was refered to this post on another thread - what is brine? and how does one use it in extractions?
swim doesn't want crappy yields
(Chief Bee)
11-03-01 01:42
No 232344
Brine is a concentrated solution of table salt in water. It is used to pull water out of organic layers, and to push organic products out of water phases.
(Hive Bee)
01-11-02 01:31
No 254949
Hi Everybody,
Man I'm really suprised to see this as a sticky thread. When I first put it up and got criticism for some of the questionalble points mentioned, it really did break my heart as I've been working on this file for a long time now (still am of course) and just wanted to contribute something back to the hive. Thanks for putting it up LT/ ... I get the sense now this compilation may be more valuable than I originally thought.
...a (aka smokemouth)
!circlesnort
(Daddy)
01-13-02 14:11
No 255904
Rhod, you remember him now? Our OldHive-threads-savier!
LT/WISDOMwillWIN
(Chief Bee)
01-13-02 20:27
No 255993
Yup, definitely. Hi Smokie!
(Junior Service Representative)
01-13-02 20:38
No 255997
An abridged verion of this, w/o benzo-wacker, in AcrobatTM, can be found here: http://www.geocities.com/thepoohbear4eve
Thank you smokie, for Project Blackbook,
PB
(Hive Bee)
01-31-02 01:38
No 262962
Cheers Everybody !
Putting this post up on the hive has definatly been my pleasure.
Having trouble linking to this geocities site referenced above though...
...a
circlesnort
(Daddy)
02-07-02 22:46
No 266620
Anybody who has a list of these sniplets, perhaps based on just ONE method, or more, is invited to post it here, lots of really precious info is hidden in just one small post of a known or unknown member, regarding a known or unknown method.
It can be priceless info for someone starting to think about trying out such a method. LT/
PS: I came to reviewing just chapter five from Archaeoptrix's long post, thought I should get some help from colleague staff members perhaps, or knowledgeable other members, like Terbium, Foxy2 etc etc.
WISDOMwillWIN
(Hive Addict)
04-03-02 20:25
No 291890
For those who are allergic to high voltages or otherwise unhandy, O3 generators can bee bought at your local hydroponics store. Theyre not cheap, but some models even have a nice 1/2 inch hose connection.Very sano. Theyre also GREAT for deodorizing/sterilizing stinky boots!!!
--back in the fray,
Bozakium
(Stranger)
04-19-02 05:30
No 298950
Zed has generally avoided stinky reactions. Zed likes room
temperature reactions, and Zed likes to do reductions with Pt and H2. However, on the rare occasions when Zed has run a
stinker (like the Leuckhardt): A two holed stopper with two
short glass tubes in it, can be loosely placed on the top
of your condenser, attach flexible tubing to one of the
tubes and attach the other end to a glass tube inserted in
a stopper in a filter flask, attach the filter flask via
tubing, to a water, vacuume aspirator, adjust water flow
so that a gentle breeze, brings those stinky gases through
your venting system dissolves them in water, and washes them
down your drain. Of course, this will be "Old Hat" to most
of you veterans out there. As for the idea of placing a bucket full of activated charcoal in the system, I hadn't
thought of that! Please note, if the reaction is also generating poison or explosive gases that are not so water soluable, you better find a way to either react 'em (HCN + KOH) or you better allow their final venting, in a well ventilated area where you ain't gonna be for a while. Naturally, your water bill will go up. But, since you will continue to be a free man, woman, or whatever, you will be able to pay it. If all this eliminating odors seems like
too much trouble to you, move near a plywood factory, these
areas sometimes smell so terrible, that the stench you are
generating might go unnoticed..............Zed
P.S. Try to use solvents, that don't stink.
Diethylether is a fine solvent. Well, except for narcosis, volatility, flamability, forming explosive mixtures with air, forming explosive peroxides; and having a distinctive, persistant odor, that can recognised 100 yards away. Other
than that, its great.