10-07-01 16:41
No 221244
Regaring post-animation process of isosass:
Thought about the situation, and it would be nice to obtain honey in solid form without having to go outdoors to gas. What would the downside be to adding dilute HCL(aq), and evaporating aqua? Melting point of honey pretty low?
If washed with acetone, then re-xtalized, would purity be equivalent?
PB
(Chief Bee)
10-07-01 16:57
No 221253
Do it the Pihkal way, dissolve the freebase in twice the amount of IPA, add an equimolar amount of conc HCl, and then crash out all the HCl salt with a lot of diethyl ether.
If you recrystallize the MDMA*HCl properly, it will take care of any impurity included in the crystals by other inferior crystallization techniques (like simple evaporation).
(Pioneer Researcher)
10-07-01 19:15
No 221279
You can neutralize the base with aq. HCl, even with the solvent, then evaporate everything till 130-140 C (mp 147-151) and add 4 volumes of acetone to the brown syrup when it cools a while, with stiring, to see the deposition of crystals, filter and wash the cake with acetone. The product is what it has to be, but is a bit smelly and depending on the quality of ketone is snow white, white off or a bit tany. All the times I've checked the mp of this product was in the right range.
As Rhodium says is a inferior techinque, more a cooking procedure oriented to save solvents and get a product with enough, but not the best quality.
(Hive Bee)
10-17-01 05:51
No 225560
Disolve freebase in 3x volume of acetone, pipette in aq. HCl until pH ~4, throw in freezer overnight wake up with a smile.
something for your mind.......
(Pioneer Researcher)
10-17-01 23:46
No 225950
Dope, that sounds really good.
(Stranger)
10-18-01 03:00
No 226010
What about the risk of formation of the imine? If it's a matter of a primary amine? E.g. amphetamine reacts with aceton in the presence of an acid (HCl) to form the N-isopropyl-amphetamine. Or with secondary amines the intermediate is formed, and is probably hard to recover. Or is this aspect negligible?
(Chief Bee)
10-18-01 03:32
No 226026
The isopropyl-substituted amine does not form unless a reducing agent is present, but I would worry about some imine formation using acetone as crystallization solvent. But if the "field testing" of this crystallization method works good for DopeAmine, then I guess that is just a theoretical worry.
(Hive Bee)
10-18-01 03:56
No 226034
Take the time to gas some MeOH with HCl to ~15-20% weight HCl. Store this in the freezer, and use this soln for your acification needs.
(Hive Bee)
10-18-01 04:31
No 226044
What can I say. I never thought about that and I never had to cuz it was never an issue. I'm surprised that what I said was anything new around here. I've mentioned this b4. I wouldn't recommend acidifying past 2 although I've done that b4 too. Anywayz, I've always done what I said above with good yield. Back in tha day, I used to filter the crystals and then let the solution evaporate down to crystals and goo. Then redisolve in a bit of acetone and throw back in the freezer for a second crop. But now I wanna try Rhod's method cuz that sounds like fun! So don't worry about it. It works like a charm and is great for the lazy man. It has always been my experience that when you evaporate down your mother liquor, there is always a bit of dark red/brown crap/oil inherent from the reduction. Now if someone were to say that is the same color as imine, then I'd think maybee just a tiny bit gets converted to imine but still nothing worth fretting over.
BTW I accidentally made MDEA once while trying to methylate MDA cuz I used ethanol + acid + heat (<-not sure on the last one). The GC/MS had mainly MDEA with a little bit of diethyl in there too!
something for your mind.......
(Hive Bee)
10-20-01 23:23
No 227276
or you can just neutralize the freebase with conc hcl, and pour 4x ice cold acetone or ether on it and watch the instant xtal explosion. if you like to experiment you can form the sulphate by neutralizing with h2so4 in ipa 20% and cold acetone. just remember the sulphate weights 20% more and if youre going to store it rextalise it.
j
"a peeping tom at the keyhole of eternity"
(Hive Bee)
11-08-01 01:12
No 234327
Once you have your freebase in your non-polar (acetone is NOT a non polar) you can do Dope Amine's freezer route. it works like a charm. There's no need to get the free base in acetone though. Just make a teabag full of dried epsoms and dunk into freebase/non-polar for a good 30 min. This will dry the solution so when the HCl is added, one just shakes well and cools in the freezer for 10- 15 min.Crystal mass will form on the bottom of the flask. Or if you live in a cold area, just do the HCl dripping outside...It's snowing! There's no need to GAS to reap the salt. Just try and use the highest % HCl possible. if you get your HCl through a chem supply house it's usually the 8 stuff.
Don't forget to re-crystalize with cold dried acetone (dried if possible)
Sounds like fun.... sounds like something Assrash would like to see done for REAL. But this wont happen as Assrash doesn't break the law.
Assrash only predicts that these procedures will work fine.Damn fine.Awsomely. Perfectly!!!
-Assrash Ouch!
(Hive Bee)
11-08-01 04:39
No 234411
if doing the hcl poured on the freebase route, use the 50% hcl from a chemhouse, if you can get it, then evap the acetone under a heat lamp to get what is trapped in the water, no gassing
j out
"fuck the media"
(Daddy)
11-08-01 09:58
No 234503
Totally BULLSHIT the last 3 posts!
And to the others:
Do you have only short memory?
We discussed this matter a long time ago several times, and the best solution ever found:
Use TOLUENE to mix with your DISTILLED freebase (3x more to 8x more) and neutralize with 33% HCl (=67% water in it!) or gas with 99% HCl GAS. An end pH of 4-3 doesn't hurt at all. You want to be sure that all freebase is converted to the chloride salt!
Then in case of the 33% HCl, boil off the water, filter crystals or just decant the toluene, in case of HCl gas just decant the Toluene (re-usable!), after all crystals precipitated,
then ALWAYS recrystalize your (wet or dried) IMPURE crystals by soluting in hot boiling ETHANOL or IPA (the minimum amount necessary to solute all crystals, these ALCOHOLS will keep all non crystallizable impurities soluted), and then add 3-4x icecold ACETONE (cold acetone also doesn't smell like hell!), let formed crystals precipitate, decant the alcohol/acetone off, wash crystals a few times with a bit fresh ACETONE, result: 99.9% pure endproduct.
(All extra HCl from the pH 4-3 overshooting when neutralizing your freebase will be soluted in your toluene, acetone, alcohol, so all these urban legends about burned lips and tongues, forget it!)
I'm not even going to look up the threads, should be common knowledge by now.
1. Use HCl gas (faster, cleaner)
2. If you can't get HCl gas , use 33% HCl. (In fact much safer from an acquisition viewpoint!)
Big ADVANTAGE: TOLUENE doesn't smell 1 km around your "secret" lab! LT/
PS: all these short step brainiacs drive me crazy, these are all wellknown labprocedures, any shortcut taken takes you a long way off from what is really possible in terms of purity and REAL yields.
Especially the idiots who tell me: but then I loose precious WEIGHT !
I hope you loose so much weight yourself that it becomes inpossible to multiply or set one step in a lab, stupid fuckers! LT/
WISDOMwillWIN
(Hive Bee)
11-08-01 18:46
No 234582
please LT, don't hold back, tell us how you really feel.
is it necessary to watch the pH while gassing?
also, SWIM has seen bad things while trying to gas all the salt out at once. SWIM ends up gassing the same toluene many times, a la dr gonzo's photo essay; up to 7 times on a 2x MM Nitro Al/Hg.
if SWIM tries gassing it all out at once, the salts get very dirty, a medium yellow or brownish colour. why is this?
(Chief Bee)
11-08-01 20:45
No 234608
You cannot check the pH of a non-polar solution. A good way is to have a damp pH paper above the solution being bubbled, when HCl gas escapes the solution without being absorbed by the solution, you're done.
(Newbee)
11-08-01 21:22
No 234616
Good point Rhod...SWIM had some isopropyl substituted MDA lately....could not figure out where it came from but your remark makes sense. BTW imine formation is observed by SWIM but only to a very minor extent.
I'm more curious about the things I dream than about things I see when awake!
(Hive Bee)
11-26-01 07:56
No 240638
(Rated as: excellent)
You can check the pH of acetone by wetting a pH paper, shaking the excess water off and dipping.
If you crystallize reasonably clean product from acetone or you gas DCM (for MDA) you DO NOT have to recrystallize. And my standard of purity is only the whitest of white. C'mon LaBTop, and boiling off water from toluene sounds like a bitch. Any of these methods if done right will produce extremely pure white crystals. For MDA, gassing in DCM is of course the prettiest with the big fish scales. But I believe the 2nd best method for MDA and THE BEST method for MDMA is to simply add aq. HCl to product in acetone. As far as ease of set-up and execution, I don't think anything is as easy as acetone + aq. HCl. The new improved version below was tried after the discussion of imine formation and differs from old in the temp of addition and the concentration of amine.
Light golden MDMA freebase was disolved in ~6x it's volume of acetone. It was found that making the solution more dilute than the old 1:4 was very benificial because crystallizion can occur without any cooling. The flask was placed in an icebath on top of a stirrer and the solution was allowed to rapidly stir and cool down. Next, conc. aq. HCl was slowly pippetted (really fast dripping) in repeatedly and the pH was checked with water wetted pH strips until the pH was 2-4. About a third of the way through the addition of HCl, the solution will have exploded with granular crystals (like NaCl as opposed to fishscales from DCM crystallization). The flask is covered and placed in the freezer overnight and the next morning, the solution is filtered to recover ~90-96% of the product. If the product oil was dirty then washing with a bit of ice cold acetone will clean and lighten it up. Evaporate down the mother liquor, redisolve in 1/3 the original amount of acetone and throw back in the freezer to recover the final bit of product.
something for your mind.......
(Junior Service Representative)
11-26-01 18:10
No 240800
kapten,
I understand that gassing is far less difficult than the synthesis itself; however, I would prefer to dream everything inside, never leaving untill glass is clean, and product is in hand. If SWIP uses a gassing setup, he plans on using his filter flask, with a seperatory funnel on top.
But let's not start counting chickens before the eggs hatch,
PB
(Distinctive Doe)
11-26-01 19:02
No 240832
You could gas with one of the set-ups that some use. They pump air(aquarium pump) thru conc. HCl to carry residual HCl gas via tube to gas product. Way slower but much safer, very controllable, definately need a drying tube though.
Do Your Part To Win The War
(Junior Service Representative)
11-26-01 23:47
No 240924
How slow are we talking about? Also, couldn't one gas indoors using a bong-like apparatus, where extra gasses are passed through to a hose going outside, or to a closed system aspirator station?
PB
(Distinctive Doe)
11-26-01 23:51
No 240928
Ask Dwarfer
I heard him describe it
Do Your Part To Win The War
(Stoni's sexual toy)
11-27-01 00:08
No 240938
The Stoni gassing procedure:
Plastic squeeze bottle with a lenght of clear PVC tubing attached to the screw on top. Put in some solid NaCl, add a few milliliters H2SO4, close bottle and bubble an air/HCl mixture through your solvent by squeezing the bottle. Works great. Once HCl generation slows down shake it a bit, or simply add more H2SO4.
(Hive Bee)
11-27-01 07:53
No 241124
Stonis method is the shit. No worry about smell anything. Only difference i do is attatch the hose to a jar with a lid and a fitting on top for the other hose on top. As gas is generated it slowly will fill up other container and as it comes in contact with solvent boom crystals. put a stirbar in on slow for agitation and sit back relax go out whatever you have youre crystals. Never had a problem - no equipment really needed no smell. Shit I did it in my bathroom with my wife in the other room and she never knew. Works like a charm
(Hive Bee)
11-28-01 08:39
No 241530
And you don't need aqueous HCl to gas, just drip sulfuric on NaCl.
something for your mind.......
(Stranger)
05-13-02 15:51
No 307935
This is a very interesting debate between gassing and simply adding aqueous HCl to form end product. Swim has not tried gassing but is not terribly inclined to with the success she has dreamt about dripping in ice cold (lab grade) 36.5-38% HCl into the freebase (methamph.) toluene mix and watching carefully to see when the colour equalizes between the two layers, as in their is no cloudiness in either layer and ideally the colour should be golden to golden bronze. Shake a little in sep funnel and leave to stand for around 15 min or so. If the toluene fbase mix is dry then crystal will have already formed blocking your exit from the bottom of sep. funnel. so at this point one can either filter the whole mix, or as swim prefers, add a little distilled H2O to dissolve the crystals and drain off bottom layer without any tol coming over. Putting bottom layer on hotplate to over 105oC but below 140o and directing a hair dryer at pyrex container (ideally in oil bath on hotplate) will bring the water off nicely and a skin will form. When skin is nice and thick the container is let to cool down a little and placed in fridge. After about an hour or so the mix is filtered, liquid reduced again, and the crystals rinsed with ice cold acetone. Recrystallization takes place with methanol and a splash of acetone. Awesome shardage! It has been noticed that if too much HCl is added the bottom layer will turn a darker colour heading towards deep purple at around pH 3-4. Does this hurt the yield swim wonders as it has never been actually determined quantitatively? Also, when the two layers as afore mentioned match in colour (just) and the cloudiness in both layers disappears the pH is usually 8-9 and the mix crystallizes fine, and then can be hit again cautiously with the HCl. Is one better off to stay above 7 or just below it? Anyways, whenever neutral is achieved in HCl addition results have always been favourable, but swim wonders if it is just fine to speed it up cautious wise and land where ever between pH 3 - 6.# ? One last question, what is the dark brown ultra fine sediment that changes the base colour so dark when re-extracting from say ones acetone wash or somewhere fucked up mixture? Attempts at removing it through NaOH and washes with water have been not all that great. Distillation would be the obvious answer but unattempted as of yet in dreamland. It would seem that this sediment only occurs when the pH is sent too far below neutral.
I know what I like, but I might like something I don't know.
(Hive Bee)
05-13-02 23:25
No 308098
even if you gas outside, if there is a void in wind current you're still going to burn your self if you catch a puff of HCl gas. The prefered method here is to place a cheap high velocity fan in the window, and put a couple pillows on either side and set it blowing outward. Works like a charm, all noxious gas is quickly escorted out.
Alternatly set up a distillation setup, replace condenser with column packed with drying agent. Into the boiling flask is HCl/NaCl mix - at the three way adatper between boiling flask and condenser position addition funnle containing H2SO4 - in the recieving flask place solvent/freebase. Lastly between the column and reciving flask use a vacuum adatper that has a drip tip, place a hose from drip into solvent/free base to the vacuum off nipple (nipple, teehee) attach hose running out window or into basic solution.
Can a bee be visa vis its entity when half a bee philosophically must ipso facto half not be?
(Pioneer Researcher)
05-14-02 02:03
No 308177
I've used the method of evaporating toluene+alcohol+aqHCl till 140 C because it's very easy and you can process any amount without gassing. Now I think it produces a bit of decomposition of product, actually a mix of IPA + toluene + aq HCl is evaporated with the aspirator at low temp, water is removed with the azeotropes and crystals appear in the flask, more toluene is evaporated and finally it is filtered and the crystals in the flask are taken out and rinsered with acetone. Much better, no decomposition and maximum yields.
(Stranger)
05-19-02 07:23
No 310627
Wondering a couple more things and thank you much Sunlight for swis posting a reply to swims post. What is notSunlights opinion on the ideal pH to have the toluene, isopropyl, HCl(aq) mixture at before reducing to obtain the golden key to the diamond mine, and if certain solvents ie. methyl hydrate, will work better at a different pH than the one ideal for isopropyl - (the question mark isnt working on keyboard) And secondly, swim has pondered and experimented intensely for some time on how to construct a trap that will capture low boiling solvents like acetone, isopropyl, methanol, etc. for recovery and to not eat the lining of swims many assorted pumps -- swim has wondered if possibly constructing a thermos containing liquid nitrogen in the walls or perhaps setting a pyrex filter flask trap right into a bath of liquid nitrogen, would get the trap cold enough to condense all low boiling temp. solvents and stop them from getting sucked into the pump , any comments appreciated -- Also, if swim may, can isopropyl, methanol (methyl hydrate), ethanol 95%, all be used interchangeably and even mixed perhaps, in crystallization procedure (question mark) hehehe. Swim has used them all independantly with varied success but wonders if someone could point out ad and dis advantages of the threes use.
Much is grassy ass,
R
I know what I like, but I might like something I don't know.
(Bear With Me)
05-22-02 06:50
No 312328
...and wish the best of luck to those who dream. PB'll fall asleep one of these days, I hope
PB
Put your left leg down - your right leg up,
Tilt your head back - let's finish the cup!
(Pioneer Researcher)
05-22-02 15:23
No 312450
Best is IPA, methanol does not form azeotrope with water, and ethanol forms and azeotrope, but you'll have at hand the azeotrope, not absolute ethanol. IPA forms azeotrope with water and with toluene, below their respective bp, what means that you remove the water and IPA and excess toluene at < 10 C with a poor vacuum (aspirator). And yes, the problem is that if you use it, the solvents will go to the drain. Anyway, if you distill at room temp, you can't isolate the toluene and IPA, so it could be a waste and it has some ecological concerns...
(Stranger)
05-25-02 13:30
No 313993
Many dreams have been found to include exclusion of all three mentioned solvents, but for recrystallization. When it is time for the picnic and the chili is first pulled out it is done with just HCl(aq) and a splash of H20, set to chill after slight reduction and filtered, redone until nothing left in the basket, must be Yogi. Recrystallization done with Methanol cause of ease of accessibility, cost, and odor. No real complaints as 95% comes back as large shard. So swis, you are saying that swim would get better results in recrys. with IPA or in the initial pull by omitting any splashes of H2O and sticking to HCl + IPA into the toluene for release.(question) or could it be swim is missing quality nap and not realizing recrys. may not be necessary if IPA + HCl (aq) used solely in initial (and only then) pull. Well not to bore y all so will compare with next nights sleeep. Again, just wondering what is ideal guideline to follow regarding pH. If stopped at around 8-9 , had a dream that reoccurred several times over while waiting 30 min between naps. Could this just be a waste of time though compared to just adding more HCl(aq) and H2O or IPA down to say pH 5 right off the pillow. Swim guesses that would make interesting thing to dream about comparatively as well. Hate to waste sleep so appreciate any guidance. ZZZZZZZZZZzzzzzzzz
I know what I like, but I might like something I don't know.
(Pioneer Researcher)
05-25-02 18:06
No 314048
I don't understand exactly what you say.
First, after extraction of the base and drying the solvent, you xtallize. There are many methods
1) PIHKAL evaporate solvent, dilute base in IPA, neutralize with conc. HCl and add 4 volumes from IPA of ether or acetone.
2) Same, but prepare IPA+ aq HCl and dry it MgSO4 or NaSO4. Neutralize the base directly with your acid IPA, then add ether or acetone.
3) Gass your dried solvent + amine (toluene or ether) with HCl, wash with acetone.
4) Dilute the base in 6 vol or so of acetone, neutralize with aq. HCl and put in the freezer, recover crystals, evaporate everything and do it again.
5) Add to your toluene extracts IPA and aq HCl to get a homogeneous mixture at pH 5, evaporate in vacuo (or at normal pressure) removing water, IPA and toluene, when you have a lot of crystals in the flask and some toluene, take them out, take the rest out with acetone, filter and wahs witha cetone.
6) and more and more...
Once you have your crystals, you can rxistallize to get more pure stuff (or specially if your crystals or not white) by diluting them in the minimum amount of boiling IPA, then add 4 volumes of cold acetone. For MDA use methanol.
If you make things correctly and get nothing, think about a failure in your production.
(Stranger)
05-26-02 05:02
No 314276
Please accept my apologies swiS for trying to bee too clever in swims last post. What swim was saying is that after extraction of base from reaction mixture (at this point a mix of NaOH,H2O,product,NaI and other salts(swim thinks))into 3 volumes of toluene, (so one theoretically has just base and toluene along with some impurity) all that was added was 36.5 - 38% HCl (aq) and a splash of H2O (by small swim means 50 ml or so regardless of volume in sep. funnel), however the criteria for adding the H2O is to stop the end of the sep funnel from clogging up with xtals, if the toluene is wet and no xtals are appearing at bottom of sep then no addtl. H2O is added. (had bad experience with using MgSO4 to dry cause swim was dumbass and after microwaving it, ground it into coarse powder, added it to toluene and made big gooooey mess) This bottom layer which is just slightly on the basic side of neutral is then reduced until a healthy skin covers the liquid in the pyrex tray on hotplate, at which time it is put in fridge (above zero celsius) and left for a bit. Upon return xtals have formed quite heavily and are filtered off, rinsed with acetone, dried and re-xtalized in methanol (minimum amount like swis says) with only a splash of acetone (50 ml) and not 4 x volume, will have to try that though since swim only gets two thirds original weight back each rextallization. The remaining liquid from the rextal. is reduced further and process repeated to eventually give up the aforementioned 95% original weight. What is the 4x volume of acetone for(question), is it to have greater yield on initial recrys. or is it affecting size or shape of xtals, or could it bee affording a purer end result. Overall and original point swim is trying to make here is that why use the more odorous (is that a word, hmmmm) solvents like IPA or ether when just plain old HCl(aq) and mild smelling (swim thinx anyhow) methyl hydrate seem to do very well for xtallization. Swim dont want to beat this thing to death and appreciates the patience shown 2 da rookeee.
I know what I like, but I might like something I don't know.