Newsgroups: alt.drugs.chemistry
From: [an 216208] at [anon.penet.fi]
Date: Mon, 13 Nov 1995 10:27:37 UTC
Subject: *ZWITTERION* - Final on MDP-2-P


Well kids, the ballots are in and all the votes are counted.

When we last left off, ZWITTERION was still hydrolysing the epoxide using
H2SO4 on a "simulated" steam bath. Temperature proved a bit difficult to
control, wandering between 80 and 115C. Not exactly sharp lab technique, but
THEN AGAIN, ZWIT ain't none for his flashy lab skills. Besides, the more I
FUCK up, the better chance YOU have of doing better, right? Right.

Okay, so the temperature falls in the flask and it's been 3 hours so what
the fuck - let's dump this baby into a goddamn beaker and start EXTRACTING.
Whoa there! Better chill that shit down first... nothing like having ether
contact something that's currently TWICE IT'S BOILING POINT. Yah - That'd be
pretty spectacular.

So ZWIT sets the beaker in ice water while preparing the necessary reagents
for all the washes and extractions. After the ketone/acid mix has cooled to
about 18C, ZWIT notes the color and appearance. There are two layers
present, though not entirely immiscible. A dark, almost black one is on the
bottom - the ketone layer, and a translucent reddish-yellow one is on top
(the yellow is only apparent near the glass-liquid interfaces, though). ZWIT
does the customary three-volumes of ether extraction and combines the
extracts, keeping them in the freezer all the while. A total of 225mL of
ether is used. ZWIT sets aside the post-extraction aqueous solution JUST IN
CASE!

Next comes the water wash. ZWIT uses CHILLED distilled water in two washes
of 100mL each. The wash water looks much like the aqueous post-extraction
layer, proving the wash was a neccessary step. NOW COMES THE TRICKY PART!

The final wash is with 10% Sodium Hydroxide solution, and this one is a
BITCH. Why? Because a lot of the black shit goes into the hydroxide layer,
MAKING IT INDISTINGUISHABLE FROM THE ORGANIC LAYER! ZWIT does a single wash
with 100mL of 10% NaOH, but notices that it would be smarter in the future
to do 2 or 3 washes of 50mL each. ZWIT solves the "can't-tell-which" problem
by REMEMBERING how much NaOH solution was added and holding the sep funnel
IN FRONT OF A WINDOW (bright light kids - works every time).

The organic layer was dumped into a distillation setup and the ether was
recovered for reuse using ice water in the condenser flow.

Now the vacuum pump is connected and the distillation system is taken down
to whatever the damn thing can manage. There is some VIOLENT bumping for a
minute and a little water jumps through to the receiver. ZWIT ignores it
because a little water never hurt MDP-2-P before. The heating mantle was
cranked way up for the projected 200C distillation temp and a pale yellow
begins to condense at around 180C. When charring appeared imminent, the
mantle was dropped down from around the flask and the vacuum released. It
charred anyway. Bastards!

The distillate is a PALE YELLOW OIL that smells JUST LIKE CARDAMON -
goddamn! That's a NICE bit of information to know, kids! And that smell is
the smell of MDP-2-P. Yes!

The yield of the distillate, and GET THIS KIDS, was 20.6g! Can you believe
that? To the goddamn tenth of a gram JUST LIKE SHULGIN. Maybe my lab
technique ain't so bad after all?

Oh, and just like most ketones, be careful with it and PLASTIC! A drop got
on the top of ZWIT's scale and started EATING A HOLE THROUGH IT!

Here's a quick review and chronology:

1) Fractionally distilled isosafrole - 1hr
2) Formed ketone - 24hr
   a) prep - .5hr
   b) addition of isosafrole - 2hr
   c) formation of epoxide - 14hr
   d) prep for hydrolysis - .5hr
   e) hydrolysis of epoxide - 4hr
   f) workup of ketone - 2hr
   g) distillation of ketone & cleanup - 2hr

Note - THE charring is BAD from distilling the ketone. One of ZWIT's flasks
is STILL sitting in conc. HCl 6 hours later without any sign of breakup.

Next - the MONEY QUESTION: performing the Aluminum Amalgam Reductive
Amination ala Dr. Shulgin's PiHKAL #109 - does it work for the home chem.idiot?

[END OF TRANSMISSION]
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