04-11-00 23:06
No 107752
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[Image][Image] Methods Discourse
[Image][Image] First posted 100% OTC dream (told y'all)
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Author Topic: First posted 100% OTC dream (told y'all)
Ezekiel [Image] posted 08-29-99 10:16 PM ------------------ Ezekiel [Image] posted 08-29-99 11:29 PM So what do you think? No lies or exaggerations are ------------------ equarius [Image] posted 08-29-99 11:48 PM Could Ezekiel please email moi at equarius@hushmail.com Nice work Cdn bee Osmium [Image] posted 08-30-99 12:44 PM psychokitty [Image] posted 08-30-99 07:48 PM As for your problems regarding gassing and such, you may Good luck to you in the future and keep up the good work. --PK psychokitty [Image] posted 08-30-99 09:36 PM Taken from JACS Feb. 20, 1953, vol. 75, pp. 921-925. (b)Leukart Reaction--To a three-necked, 2-Liter flask, --PK Ezekiel [Image] posted 08-30-99 09:56 PM Os- what suggestions do you have. BTW, biological test dreams were amazing. ------------------ Ezekiel [Image] posted 08-30-99 10:44 PM Searched all microwave articles, none on the Leuckart ------------------ psychokitty [Image] posted 08-31-99 05:30 PM Anyway, the thread you are looking for is called "Son of --PK daragh [Image] posted 09-01-99 03:28 AM hellman [Image] posted 09-01-99 08:07 PM Your're on fire Ezekiel, How do we make n-methyl formamide to go on to mdma?. cool man, well done! hellman psychokitty [Image] posted 09-01-99 09:26 PM --PK Ezekiel [Image] posted 09-01-99 11:00 PM ------------------ psychokitty [Image] posted 09-02-99 06:29 PM --PK dpHarma [Image] posted 09-03-99 12:59 PM fascinating report! couple questions. 1. did you use the 65% acid 'straight' from the jug? was 2."He adds muriatic acid till the solution is pH 8. This thanks for the inspiration dpHarma Ezekiel [Image] posted 09-03-99 03:14 PM And I'm going to have to go back on my word... MDMA is a ------------------ Atomicdog [Image] posted 09-04-99 11:55 AM psychokitty [Image] posted 09-05-99 01:51 PM That was rather long winded. But I'm sure you get the --PK Atomicdog [Image] posted 09-05-99 04:27 PM The more i look at this the more i wonder why the leukart If I did that sort of thing, I'd work this bad boy up and lets talk more PK, hellman [Image] posted 09-05-99 07:46 PM I feel the same way,. Ezekiel, To not make homemade Hg salts, refer to the thread hellman I sometimes wonder about making formamide from formic Ezekiel [Image] posted 09-06-99 04:56 PM A 100% OTC MDMA synth is about a week or two away, Thanks everyone for the encouragement. ------------------ hellman [Image] posted 09-09-99 01:20 AM I'll race you for a good n-methyl-formamide synth. Goodluck, hellman Atomicdog [Image] posted 09-09-99 06:25 PM I say again, this may prove to be THE method for hacks I'm working up a procedure with scaling from all the refs AD hellman [Image] posted 09-09-99 10:35 PM Does anybody know if water eill fuk with this? hellman Administrative Options: Close Topic | Archive/Move | Delete Topic Contact Us | the Hive Powered by: Ultimate Bulletin Board, Version 5.39a
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The following is all a dream and never actually happened
in real life:
Ezekiel decides to make MDA
First he takes some sassafras oil and rigs up a simple
distillation with a fridge vacuum pump. He throws away
the first stuff. When the distillate looks and smells
right, he collects 70 g. The leftovers are dark red, the
distillate is clear and smells like heaven. Oh baby!
Then he adds 7.5 g MgO and 0.7 g KOH, and heats it to a
boil for 15 min. At this time is it brown and full of
white and brown particles. After cooling, he add a bunch
of water, but the solids do not want to dissolve, and he
gets the most horrible emulsion on the planet. So he lets
it sit a while, and decants onto a vacuum filter with
qualitative paper. Lots of crap goes through and the
paper gets plugged immediately. Argh! Next time, let it
sit overnight and filter through cotton I think... He
washes the iso with water till its pale yellow, and plays
around with the solids for a while. Anyway he finally
ends up with 40 g iso. What a mess.
Then he adds 125 mL DCM and 3.75 g Na2CO3 and starts
stirring in an ice water bath. Over an hour he drips in
32 mL 35% H2O2 mixed with 72 mL 65% formic acid. He
assumed they were both v/v when calculating moles. Was he
right? Since the formic was a little more dilute than
normal, and the sirring was poor (the magnet kept jumping
around) he let it stir for 48 hrs. He then separated the
layers, both orangy, and distilled the DCM off of the
organic layer. To the residue he added 380 mL water and
started stirring. Then he added 40 mL 95% sulfuric acid.
He didn't premix cuz the heat generated boils away the
last traces of DCM. He heated the mix to 75 oC for 2 hrs.
The oil was then a dark red. He extracted with DCM,
washed with saturated bicarbonate, and distilled. When
the distillate started to get a bit orangy, he stopped.
The MDP2P was thick and yellow with the slightest green
tint. Smelled faintly like pepper and burnt wood, but
sweeter. He got 20.5 g. That's only 46.5 %, but there are
a lot of things he could have done more carefully, and
there was not one reagent grade chemical involved, so not
bad eh?
Then he decides to make some formamide. He takes 200 mL
65 % formic and adds household ammonia to pH 8 (1875 mL)
and puts this in a huge glass pot. He boils it for HOURS
until the smell changes from ammoniaish to hellish. There
was only 80 mL left and there should have been 150.
Doesn't formamide decompose below its boiling point?
Shit. Oh well, he says, the next part uses a seven-fold
excess anyway.
So Ezekiel takes his 80 mL of thick, yellow (huh?)
formamide and 20 g MDP2P and adds 10 mL water and 1 mL
glacial acetic acid. He heats this to 150 oC. After six
hours there is only 7 mL distillate. Strange. When it
separates, the oil is dark red. He extracts it with DCM,
washes with NaCl(aq) and distills off the DCM. Mmmm, red
goo.
Then he tries to mix up 27 g NaOH, 125 mL 99% IPA, and 31
mL water. This forms tree layers. White IPA on top, then
undissolved NaOH, then really hot, clear water. Oh well,
make a slurry he thinks, and adds it to the goo and
refulxes for 45 min.
At this point ol' Zeke does what I think a lot of new
bees do. He realizes that he just made X but it's in a
flask full of crap and he panics. He has never tried MDA
before and he really loses his cool and strats to goof up
a lot. So he adds some water to dilute the base, and
vacuum distills _most_ off the ethanol. (A bunch bumps
and goes out through the vac line. Ezekiel cusses
uncontrollably.) Then he extracts a few times with DCM,
and washes a few times with water. He's left with a dark
red DCM solution. What to do? He has had very bad
experiences with the gas; Logical's sulfate method sounds
appealing but probably won't work in DCM; Sunlight's
method also sounds good but the solution is REALLY dark
red; Strike and Chem Abs. say distill, but Zeke is afraid
he has such a low yield that he will lose it all to his
enormous glassware. So this is what he does.
He adds muriatic acid till the solution is pH 8. This
boils away a bunch of the DCM. This he extracts with
water. DCM layer is still dark red, water is cream
coloured. Oh baby, here's where it gets good! He rigs up
a double boiler and starts to evaporate the water layer.
Maybe there's some salt in it you think? He gives it a
taste. ARGCHHH! WOO HOO! It's not salty. Its the best
horrible taste in the WORLD, amphetamine! In about and
hour the pan in full of spaghetti-like crystals, cream
coloured. He crushed them up and weighs. 9.5 g baby!
Unless you have done something like this before, you have
NO idea how good it feels to succeed for the first time
(by a new method at least). He washed them with sub-zero,
pre-dried acetone. It turnes oh-so-slightly pink and
leaves behind a mountain of snow. Lucious. This is about
a 35 % yield, more than he ever got with Al/Hg. Ezekiel
is very very happy, even though you are all thinking your
way is better. Ezekiel knows he can improve his method
and his technique to over 50 %, which is fine in his
mind. Sassy's cheap and abundand where he lives.
Then I suddenly awoke from this dream and thought holy
shit, Ezekiel, I whish I was really you and this wasn't a
ficticious dream.
So what's the point? What's the verdict? Lessons learned?
1. Never be afraid to try new methods. It's easy to think
one is the best if it's the only one you've tried.
2. Piss on reagent grade chemicals.
3. Yield is not as important as saftey, ease, and
reliability.
4. Piss on MDMA.
5. Don't be afraid of emulsions. Better to shake good,
wait a while and get all the goodies.
6. Leuckart RULES!
7. Next time distill the formamide, do a better cleanup
of the iso, do more thorough extractions and transfers,
and be wary of the evil bumping.
8. Always be patient, careful, never panic, and save
everything.
9. Even if others diss you, try your own ideas.
10. Beg others to help you even if they know you are an
idiot and they are tired of answering your stupid
questions. How about some suggestions now?
Props out to those who made this all possible: Osmium,
Rhodium, Elusis, Logical, LaBTop, Sunlight, BrightStar,
Psychokitty, the list goes on you know who you are.. and
of course, the queen bee herself who wrote the book that
made it all possible, Strike.
Never give up, y'all.
Ezekiel Out.
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Ooops. Sorry guyz. Ole' Zeke seems to have forgotten to
say where he dreamed of getting all this stuff without
ever even contacting a dangerous chem shop. So here goes:
sassy: essential oil shop in Ontario, no questions, no
names, pick-up ($100 per kilo)
MgO: health food store, in a bottle labelled Magnesium
Oxide Powder (cheap)
KOH: take KOH drain cleaner, boil till it gets thick,
then put it in the fridge; BANG! a zillion KOH crystals
(cheap)
NaOH: Gillet's Lye (hardware store)
filter paper: science store (crazy expensive)
DCM: distill from paint remover
sodium carbonate: bake some bicarbonate for an hour and
weigh the difference to make sure you lost the right mass
35% H2O2: hydroponics store (cheap)
65% formic acid: tanning shop or bee supply (cheap)
95% sulfuric acid: "Professional Plumber's Drain Cleaner"
at Home Deopt (cheap)
3% white ammonia: grocery store (cheap)
glacial acetic: photo store
NaCl: are you an idiot?
MgSO4: bake some epsom for an hour (cheap)
99% IPA: grocery store (cheap)
glassware, hotplate/stirrer, thermometer: science store,
surplus store, used labware store (price varies wildly)
vacuum pump: used fridge compressor (cheap)
involed (except calling IPA ethanol in the previous post;
we're celebrating a bit here, okay?).
Ezekiel Out.
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Very nice. Think I'll not try the Leukart also.
or post yours.
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Congratulations! Well done. There might be a few minor
mistakes in the practical lab work, but it's the success
that counts. You got your honey and that's the only thing
that is important.
Member
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VERY well done. I am impressed beyond description.
Considering your newfound interest in the Leukart
reaction, however, you may wish to consider doing
experiments using a microwave as the heat source as
detailed in a post long ago. As I remember it, the
reaction scheme was the same, but everything was
performed in a microwave with the results being a five
minute reaction time and a yield in the range of 80-90%
with no tar formation. Since it appears that sassy will
be available in your locale for quite some time, you
could really do the Hive a favor by conducting research
in this area.
wish to give my OTC anhydrous HCl gas generator a shot.
Details of its construction and operation can be found on
Rhodium's page.
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Thought that you might find this interesting:
fitted with a dropping funnel, a thermometer reaching to
the bottom, a stirrer and a Friedrich condenser arranged
for downward distillation was added 315 ml of 28% aqueous
ammonia. To this stirred solution was added dropwise 264
ml of 90% formic acid. The stirrer was removed and the
solution was heated gradually over a 2 to 3 hour period
to 160 deg C, the temperature being regulated so that
fairly rapid distillation took place. After cooling to
110 deg C, 164 g. (1.0 mol) of o-methoxyphenylacetone was
added and the mixture heated at 160-170 deg C for 5
hours. At the end of 2 hours the upper layer of the
distillate was retured to the reaction. After standing
overnight the homogenous solution was heated 2 hours
more. It was then cooled to 70 deg C, 360 ml of
concentrated hydrochloric acid was added dropwise and the
mixture heated for 6 hours under reflux and allowed to
stand overnight. The suspension was diluted with 600 ml
of water and extracted with benzene. The aqueous layer
was basified, extracted with benzene and the residue from
the benzene distilled under an atmosphere of nitrogen;
b.p. 118-122 deg C at 11mm, yield 95 g. (58%).
Member
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Thanks PK. Now THAT is the kind of feedback I need. Wow.
I was assured by someone that the formamide could not be
generated in situ. Will have to dream.
Please don't tell me to gas. I will next time.
Ezekiel Out.
Member
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Sorry, I reread that and it's not really in situ, it's
just in the same pot before the reaction.
I talk too much, too fast.
found. I'm really interested now though.
Ezekiel Out.
Member
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Using the Hive's search engine doesn't always work. Ever
since the last crash, there has been considerable trouble
experienced by many bees while attempting to locate
threads using keywords or phrases.
Leukart arises to battle the evil Narc hordes" by Cherrie
Baby. There were ten posts to date with the last one
being on 12-11-98 at 5:37 a.m. Oh yes, the thread can be
located under the Novel Discourse section of the Hive.
You'll have to access all of the topics from the last
year in order to get to it, but that really shouldn't be
all that much of a problem.
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Nice one ,And i'm just about to do my weekly grocery
shopping. Me thinks i'll be picking up a few extra otc
goods.
Member
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Was in the area, so just popped in to say..
I take my hat off to ya!.
This is the kind of shit we want to see.
Fuck Hg salts,
Although one question still haunts me.
I would like to see that.
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Why not just reduce the N-formyl-MDA that is formed in
the first part of this reaction catalytically or with a
hydride to MDMA?
Member
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CATALYTICALLY? Got a reference for me?
No hydrides at Home Depot this week. :-)
Ezekiel Out.
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Catalytically?: In other words, using Pd/C or Pt/C and
hydrogen under pressure.
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Zeke
it from bee-keeper's?
(SWINM found when distilling from the jug the first time,
lots of crud was left behind in the flask)
boils away a bunch of the DCM. " is pH 8 correct? the
heat of adding the acid boils the DCM away?
"this he extract with water"
so you have a two phase sol'n (DCM/prod and conc. HCl) w/
the pH of the aqueous layer slighly basic by
under-neutralization?
then add water to 'dilute' the aqueous layer and
separate?
is the layer still pH 8? when you boil off the liquid?
Member
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dp,
My mistake. Should be pH 5, which would make a lot more
sense. And yes, adding muriatic heated the solution
enough to boil off some DCM.
Untouched beekeeper's formic was used, but will be
distilled if Ezekiel dreams again.
MUCH could be improved. This was just a test.
LOT better. All Zeke would need is an OTC HgX source and
we're off to the races on that one too!
Ezekiel Out.
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Kitty - Could you please expand on how to adapt this
simple little reaction to produce MDMA? The leukart is so
easy, this could really ressurect the dreams of an old
bee.
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There really is not much to it. N-formyl-MDA is the
intermediate that is formed from reaction of formamide
and MD-P2P. If one hydrolyzes this using HCl of NaOH
solution, one will get MDA. But if one reduces the
N-formyl-MDA instead using lithium aluminum hydride or
Pd/C and hydrogen or any of the other newer ways of
reducing amides, one will get -- as a result of the
reduction of the carbonyl group on the amide skeleton --
MDMA. In PIHKAL, I believe that Shulgin synthesizes MDMA
from MDA by first formylating MDA and then reducing it to
MDMA. In this case, use of the leukart allows you a
direct way to the N-formyl-MDA.
Basically, you would make use of Shulgins second
reduction step to get your product.
picture. And if you don't, I'll be happy to try to
explain everything again.
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Hmmm... it seems to use some chems that would require a
supply house, and some experimentation(isolating the
M-formyl MDA, etc...). the other problem is buying
LiAlH4, is that a watched chem? Probably, so whats the
best way for a hack like AD to proceed in terms of chems
needed and rxn touchiness?
isn't more popular. It's realatively easy, needs no
exotic chems, and doesn't screw around with mercury!
lovely.
start converting the masses.
AD out
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Atomic Dog,
called, Hg and it's salts, by Moi!.
Or just grind together some iodine and mercury from a
thermometer. Add excess iodine to convert all the Hg,
then evap the excess iodine off in the dark, in a warm
place. You will see a fine scarlet sand remain, It's
beautifull, as far as hg salts can be that is!.
What's mda like anyway?
acid and urea, as posted by everyman, one would think
that you would need a lot of cuso4 to firstly obtain
close to 100% formic acid.
Member
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To add to the long list of opinions, MDA seemed great at
first, but after a few tries, I'd have to say MDMA is
better.
MDA's cool cuz it's easier to not make, and after it
comes on, it's really good for about an hour, like MDMA
without as much magic, but then it lingers on forever
with a really amphetamine-edge. Comedown is a LOT
smoother than MDMA, but I seem to get a bad hangover from
MDA, none from MDMA. Taking a lot of MDA >150mg gives
great visuals, but more hangover (for me anyway). I'd say
a hit of MDMA and then another half-hit an hour into it
would be my personal favorite. For jaw clenching, I suck
on DXM lozenges - it may reduce wear and tear on the
neurotransmitters.
because it needs to be not-tested a few times first.
Ezekiel Out.
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Unless I beat you to it,.
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Ezekiel-
Are you sure you made formamide? I read in the 'son of
leukart' post that Formic acid + ammonia produces
ammonium formate. I don't have my Merck on hand, so I'm
talking out my ass, but if ammonium formate is a stable
solid then that may be even better from a ease of use
standpoint.
In that same post I read that formic acid + urea does
produce Formamide, but, if formamide is unstable as you
said(again, no Merck!) then screw it! Stay with ammonium
formate, its only 2% to 10% yield diff which is
negligible if you can get 50% from this.
and pros alike if the microwave thing works out. The real
successor as champ over the Al/Hg. I LOVE no mercury man!
I can find on this, but there really should be a
formamide/ammonium formate snyth section on Rhods page,
I'll email him.
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If you could get 100% formic, say via drying with cuso4,
The Urea+formic. would be the way to go.
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(Hive Addict)
02-05-02 23:17
No 265621
Yes, he added the distilled safrole to KOH with the magnesium to dry it. Then heated to boil (reflux). That would make isosafrole.
It is cleaner if you omit the magnesium, and use a vacuum while refluxing several hours (6-8).
It looks like he used washes to clean it, but distillation is preferred, under vacuum or not.
Real men cook naked.
(Stoni's sexual toy)
02-05-02 23:23
No 265626
Also, MgO cannot be considered a drying agent. But it should clog your filtration pretty well.
I'm not fat just horizontally disproportionate.
(Hive Addict)
02-06-02 00:32
No 265645
I just want to acknowledge that Ezekiel was one of the old bees that I looked up to at the Hive. Hats off to him, I hope he's doing well! Chromic loves your ingenuity.
Anyways, he made a mistake in making his isosafrole. He should have omitted the MgO, maybe he thought it would be a good substitute for CaO, anyways, he should have left it out.
Also he made a mistake in making formamide. He should have used a vigreux column when distilling down the water off from that large volume, then once the liquid gets to about 150C, he should have then concentrated (and perhaps distilled) it using an aspirator vacuum.
HoH, here's a synopsis (in chronological order) of what Ezekiel did so you can follow his post:
1) distilling sassafras to safrole
2) safrole to isosafrole (KOH/MgO--again, do not use MgO!)
3) isosafrole to mdp2p via performic
4) makes foramide via household ammonia and formic acid (vigreux column, distill out all water using vacuum)
5) mdp2p to mda via Leukart
6) MDA to MDA.HCl via an acidic water extraction
(Hive Addict)
02-06-02 05:24
No 265743
The reason he chose that method is because everything was OTC. PdCl2 and benzoquinone were a bit more obscure back when he wrote that... Bright Star hadn't yet posted his dreams re:the wacker...
(Junior Service Representative)
02-08-02 05:03
No 266736
Or just grind together some iodine and mercury from a
thermometer. Add excess iodine to convert all the Hg,
then evap the excess iodine off in the dark, in a warm
place. You will see a fine scarlet sand remain, It's
beautifull, as far as hg salts can be that is!.
PB
(Hive Addict)
02-08-02 06:21
No 266760
Distilling sulfuric acid is nearly impossible. I've tried it before... good luck.
65% formic acid can be distilled to remove non-volatiles, and apparently it works well.
(Stoni's sexual toy)
02-08-02 11:20
No 266867
> Can someone please describe the odor.. I have nothing to
> refer pungent to.
It stinks.
> How would you seperate the two via distilliation?
You can't.
> I suppose you wouldn't really have to if water was the
> only other thing in it...
Correct.
> Wouldn't it burn you if you put it on yourself?? Ahhh!
Yes. Ahhh! As in ouch.
> Maybe give you a fake a tan!!?? Hrmm.. Am I close?
No. This has nothing to do with suntan. It will destroy your skin if left there for a while.
I'm not fat just horizontally disproportionate.
(Stranger)
02-08-02 11:22
No 266868
I suppose you wouldn't really have to if water was the only other thing in it... Im just not picturing what it would look like if accuired from a tanning salon..
What... no you silly billy not a tanning salon (Where people get all suntaned)
But it is use in tanning hide/leather... now thats something completly different...
Don't wander into a Tanning (Suntan Shop) and ask for formic acid....they will look at you blankly
I love the smell of Ketone in the morning.