Newsgroups: alt.drugs.chemistry
From: [an 216208] at [anon.penet.fi]
Reply-To: [an 216208] at [anon.penet.fi]
Date: Sun, 12 Nov 1995 22:17:13 UTC
Subject: *ZWITTERION* - On making MDP-2-P


Due to the RESOUNDING SUCCESS experienced making Isosafrole, ZWITTERION
pursued the NEXT STEP, which is to form the ketone, MDP-2-P.

Now, old ZWITTERION always thought that reacting a peracid with a
non-terminal alkene would make an epoxide, and hydrolysis of said epoxide
would result in a 1,2-glycol - but then again, ZWITTERION don't know shit.

So, ZWITTERION opened up PiHKAL to synthesis #109, courtesy of Dr. Shulgin,
and tried to interpret the SPARTAN DETAILS into a workable PROCESS.

Here is what has happened SO FAR:

ZWITTERION diluted ~20mL of 50% Hydrogen Peroxide to 32mL of 30% Hydrogen
Peroxide with distilled water.

ZWITTERION poured 133g of 90% Formic Acid into a 500mL RB flask situated in
a cold water bath on a magnetic stirrer then added 17mL of distilled water
to make 150g of 80% Formic Acid. Is there something fishy with that math?
Probably. Fuck it.

The 30% H2O2 solution was SLOWLY added to the HCOOH with stirring and
allowed to chill for 30 minutes.

32.4g of Isosafrole was dissolved in 120mL of fresh-from-home-despot(c)
Acetone (I always like to have a wild-card reagent just for fun) and this
was loaded into an addition funnel which was then placed onto the RB flask
and allowed to drip at 1 DROP PER SECOND.

All 120mL was delivered within 2 hours with temp checking every 15 minutes
to make sure it wasn't getting too HOT. The temp never climbed above 35C as
long as ZWITTERION kept adding a few pieces of ice here and there.

The color of the reaction is the KEY OBSERVATION in this process, since
these are the ONLY DETAILS Shulgin gives! Here's a list of the observed
color changes at various points in the addition:

~15mL: a slight yellow tinge.
~50mL: definitely orangish
~100mL: kind of a clear reddish
~120mL: looks like transmission fluid; deep red but clear.

The solution remained on the stirrer MUCH TO THE DIFFICULTY OF ME TRYING TO
SLEEP for an additional 14 hours. The color remained as it did after all was
added and the temperature was STABLE the entire time as noted by my DATA
LOGGING thermometer.

In other words: SO FAR, SO GOOD.

Now the setup was changed to distill on the heating mantle using a cold
water condenser and VACUUM from a VACUUM PUMP. Shulgin sez: "distill till ya
get about 60g of residue". Whatever that means, so ZWITTERION distills under
vacuum (dunno how hard a vacuum, but not out of the reach of a water
ass-pirater (c)-POPeye) until he THINKS he has 60g. The temperature started
at about 37C and climbed to 45C when I disassembled the setup to weigh the
mother liquour. It still had the noxious odor of Formic Acid and when thin
was a distinct yellow-red color. The mother liquor weighed 88g so ZWITTERION
fired up the distillation again and let the temp reach 53C this time. Upon
this second weighing, the mother liquor was much less smelly, but still with
a faint odor of HCOOH, and now weighed 44g! GREAT! WHERE DA FUCK did that
other 16g go? The distillate was still clear, so I can only assume SOMETHING
FISHY happened. Maybe Shulgin just has better lab technique than me?

To this was added 50mL of methanol (not 60 because I had 70% of the expected
yield) and ~250mL of 15% Sulphuric Acid (41.5g H2SO4 + 233.5mL water).
ZWITTERION placed a thermometer & therm. adapter into the flask and heated
GENTLY on the mantle to SIMULATE a steam bath, which ZWITTERION has NO
INTENTION of ever using! I was shooting for around 80-90C but the temp
quickly hit 115C within minutes, so I dropped the heating mantle down from
the flask and continued stirring in the free air. When the temp dropped back
down to about 80C, the mantle was replaced and set at a lower setting, where
it slowly climbed from there to 95C over the next two hours. In the next 15
minutes, though, the temperature began falling, indicating, at least to this
old bastard, that the reaction was coming to a PEACEFUL close.

Less than an hour left, I'll let you know what happens in the next edition.

[END OF TRANSMISSION]
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