Newsgroups: alt.drugs.chemistry
From: [an 216208] at [anon.penet.fi]
Date: Sun, 19 Nov 1995 16:39:17 UTC
Subject: *ZWITTERION* - Reductive amination MDP-2-P -> MDMA


Holy SHIT you've gotta be FAST with this one.

First, let's start with making the aluminum almagam - IT SUCKS!!! I am
relaying the experience from TRY NUMBER TWO because try number one turned
into a MONUMENTAL fiasco. Charred mess, lot's of ruined product down the
drain. OH THE TRAGEDY! Other than that, though, it's a very nice process.

Do not, I repeat, DO NOT make this until you have EVERYTHING ready to go!
Line up ALL your little beakers with all your little reagents pre-mixed and
THEN YOU CAN START MAKING THE ALMAGAM!

Why? THE SHIT WILL CATCH ON FIRE! God almighty can I make it through a week
without a fire??? I've had to refill the extinguisher TWICE already, and NO
IT ISN'T HALON! What will I tell the landlord???

Anyway, so the nun says to the priest, "5 bucks, same as in town". No,
wait... Aluminum. Yes, Aluminum.

So ZWITTERION has assembled 34g of MDP-2-P, which, upon scaling Shulgin's
reaction using a nice little spreadsheet eleusis sent me, meant 26g of
Aluminum needed to be cut up into little 1 inch squares. Scissors were
considered and abandoned in favor of ripping the living hell out of the
crap. You won't BELIEVE how much Aluminum foil is required to make 26g! God!
I must have been tearing at the shit for 30 minutes!

So the Aluminum gets dumped into a plastic bowl, god forbid you almagamate
mother's silver serving bowl, and approximately 900mL of water was added.
Next, .6g of Mercuric Chloride was dissolved in 300mL of water... well,
almost dissolved. The SHIT DOESN'T DISSOLVE. Oh well. It was stirred BRISKLY
and dumped into the plastic bowl. The whole sloppy mess was stirred for
several minutes while watching the news - say, nice job those Serbians have
done. After 5 or so minutes, the water starts to turn gray and little
fizzies are heard. Stirring is continued for 30 more minutes, occasionally,
while ZWITTERION measures out the remaining reagents:

38.5g methylamine hcl in 39mL water
93mL 25% sodium hydroxide soln.
340mL Isopropyl alcohol

The almagam gets toasty warm, and starts steaming. I pour the methylamine
hcl solution onto it which does nothing. Then I dump a hundred mL's of the
IPA on it, it calms down a bit. Next comes the MDP-2-P, a little IPA in the
container for rinsing, the NaOH solution - whoa that's a scorcher - and
finally, the remaining couple hundred mL's of IPA. I mash the Al-Hg down
with a Nalgene(tm) plastic stirrer and commence stirring. The temperature
climbs up rapidly and as it passes 50C I submerge the lower half of the
plastic reaction cylinder into cold water. The temp stabilises at 55C -
whew! Just in time.

The Al-Hg has a nasty tendency to rise up above the solution surface forcing
me to babysit the damn thing. I stir periodically, not really sure if this
is supposed to be a true phase-transfer type of reaction or not, because,
clearly, there are two phases forming when unperturbed. Shulgin doesn't
specify, so I opt for periodic stirring, figuring it will only be
half-fucked up if I'm wrong.

After an hour of this, the reaction temp falls from it's stable 55C down to
about 35C, but every time I stir it, it jumps back up to 45C. Shulgin sez
the reaction is done when it hits room temperature, but he didn't say
anything about the temperature jumping while stirring. Fuck it - I'll let it
sit all night if I have to, because god-damn, I expect to get 26g of MDMA
out of this!

4 hours later, the shit is STILL hovering at 35C, and bubbling like a
mini-volcano every few minutes or so. Very bizarre stuff, but not even
something as mindlessly fascinating as this can hold ZWITTERION's interest
for long, so I go to a bar for a couple of stiff drinks.

After 7 hours total elapsed time, the temp is at 27C, the waters are calm
with a delicate amber tint, much like apple juice. A small amount of
turbidity is present, so it isn't quite the "clear yellow overhead" that
Shulgin describes. Great, it's probably contaminated with MPTP or something.

ZWIT decants the overhead and filters on the vacuum buchner. Next, 25 mL of
Methanol is added to the sludge and half is filtered. The paper is changed
and 25mL more MeOH is added for filtering the remaining half.

The total filtered solution is then distilled under vacuum. The temperature
rises from a start of about 37C to 53C where it stays for SEVERAL HOURS.
There is A LOT of liquid that must be removed from the mixture, so be
prepared to spend a LONG time at the vac. pump. BTW - ZWIT estimates his
pathetic pump to be pulling a GODDAMN WORTHLESS 80mm Hg, assuming the
highest boiling fraction to be stripped is water. After a total of
approximately 8 hours distilling, there remained 55g of a reddish-yellow
liquid with some water and perhaps 10g of what appeared to be regular old
table salt. I wasn't about to sprinkle any on my dinner, if you know what I
mean.

ZWIT only has 2 250mL Sep funnels, so the next part of the process was a
REAL TREAT, lemme tell ya. The reddish liquid was dumped into a half-gallon
apple juice container which contained 1.54L of distilled water. ZWIT then
did a Tag Team no-holds-barred elimination match with his two sep funnels.
The suspension was first acidified to pH 5 using 10% HCl. It took
approximately 100mL to get it there. Next it was washed by successively
treating 7 225mL portions with 2x15mL of methylene chloride. After this
strenuous TEDIUM, ZWIT had a cigarette break - to fully enjoy the
carcinogenic methylene chloride vapors that were assuredly in the air.

Next the washed suspension was basified to pH 9 by the addition of
approximately 75mL of 10% NaOH. The suspension turned white with just a
slight tinge of pink. Also, on the bottom there was a thin layer of
PRODUCT!!! Now kids, it's time to have a little chemistry lesson as to WHY
Shulgin likely specified methylene chloride as the organic solvent here:
Because it is denser than water, and so is our product. This means that
there is no wish-washiness on whether the organic layer will go to the top
or bottom of the sep funnel depending on how much dissolved product is in it
- it will always want to go to the bottom!

The 7 deal thing was repeated, except using 2x20mL portions of methylene
chloride to extract into.

The MDMA-laden methylene chloride, a distinctive clear red in color, was
then distilled on the heating mantle with an ice-water condensor flow to
strip off the solvent. The temp stays dead on 40C for a little over an hour
and solvent removal is stopped after the temperature FALLS (no more vapor
coming over, kids). Yield of oil is 24g - hey! Where'd the other 2 grams go
to??? Oh yes. I almost forgot - this is the BASE, not the SALT. The salt
will weigh heavier. Okay.

ZWIT always wondered why Shulgin went to the extra trouble of distilling the
MDMA oil that remains after stripping the solvent. It's just asking for
trouble in my book, especially if you don't have a good vacuum pump, like me
(poor things' been subjected to every corrosive substance on the planet,
just about). ZWIT added 100mL of IPA to the flask, swirled, then dumped the
red liquid into beaker. ZWIT is about to find out WHY you distill the product...

Next is crystal-forming time! Are we EXCITED yet or what??? Boy this sure
beats making cyanogen bromide any day of the week.

ZWIT adds 10mL of concentrated HCl (muriatic acid - if it's good enough for
cleaning concrete, it's good enough for drugs) to the beaker while swirling.
There is quite a bit of fuming, but no crystals form!?!? Puzzled, ZWIT adds
200mL of ether, and now there is a dilute solution with still no crystals
forming. ZWIT suspects one of two things here: either the water content of
the IPA (9%) or the water content of my well-used ether (it's assuredly no
longer anhydrous) is the culprit, or it's because I didn't DISTILL the
goddamn shit like I was supposed to. Awwwwww jeez don't tell me I have to do
an acid/base extraction on this shit and DISTILL yet again today?

ZWIT, wanting to avoid this as much as possible, evaporates off the solvents
to leave a syrupy reddish-brown liquid that smells RIGHT, but doesn't LOOK
to healthy. This liquid was then poured onto a glass dinner plate and set on
top of a frying pan with boiling water to get it nice and toasty warm for
about an hour. The plate was removed and set to cool on the counter, SLOWLY.

The next morning, there were CRYSTALS. Of course, they were somewhat
brownish and not at all "sellable", but some judicious washing can take care
of that problem.

Total yield of crystals, pre-purification: 28.4g!
Total yield of crystals, after Et2O wash:  27.0g!
(2x25mL Ether was used)

The crystals were a light brown and had just the right smell: a hint of
cardamon mixed with amine! Ahh the JOY of home COOKING!

Kids, if you want to try this yourself, remember, it's a GODDAMN FELONY AND
A HALF! But, please, learn from my MISTAKES and then you might REVEL IN MY
SUCCESS!

Next on *ZWITTER-ALDO* - ZWIT reveals some shopping tips with surprising
name brand products with DOUBLE LIVES. OTC Solvents? Fuck THAT, we're
talking OTC REAGENTS!

[END OF TRANSMISSION]
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