posted 02-13-99 08:32 PM         

Began experiment with 30ml of "100% pure sassafras oil" (S. Albidum).
The sort any normal, law-abiding citizen might use as a pleasant
aromatic oil to relax at the end of a long day... but the use this
demented drug had in use for this innocent oil was far more insidious.

The oil was washed with 2x the volume of 28% acetic acid. The cloudy
acid layer was separated and discarded. The solution was then washed
twice with water, the first wash was slightly cloudy, the second not
at all.

To a flat-bottomed flask was added a teflon stir bar, 55ml of DMF
8ml water, 17g b-benzoquinone and ~ 300mg of PdCl2. Mixed intimately.
(picked the best looking benzo-Wacker from TSII and scaled it down
for aprox 25g of safrole).

Unfortuantly for this would-be felon, there was an accident and
some of that precious safrole-like oil was spilt. Doh! Only ~18ml
remainded. The remaining 18ml was added to the stirring mixture over
a 20 minute time interval

The solution was initially a strong red from the benzoquinone (oh, do
not get this stuff on your skin, it WILL NOT come out!). As the
maybe-safrole was added, the flask became progressively darker
brown.

By T+1:10 there had been a dramatic color change, much darker, and the
flask was warm to the touch. Cool. By T+2:45, the flask was beginning
to cool down (having reached an earlier peak in temp. of pleasantly
warm). By T+4:00 flask was back to room temp.

At T+5:00, The now-black contents of the flask were dropped into
500ml of chilled water and stirred thoroughly. When stirring
ceased, a black precipitate quickly formed on the bottom.

When the reaction was next attempted, this precipate was filtered
out as the solution was added to the chilled water. This made life
oh-so-much easier later on.

But now there's 750ml of black/red water/gunk sitting there.
Extracted 3x with 30ml portions of ether. After the first
extraction, the whole mess was then filtered to remove almost all
the black precip. and things went much smoother.

The approx 100ml of ether is a straw yellow, one might say it has
a hint of green, one might not. Entirely free of particulates. The
ether was placed in the freezer overnight (well sealed, naturally).

In the morning some dark red oil had precipitate from the solution.
The rest was decanted. This may or may not have been the right thing
to do. The ether was evaporated over a period of days in the atmosphere.

A solution of sodium bisulfite was prepared. I can now say with
certainity it was far from saturation, but apparently that really
wasn't a problem.

Some of the bisulfite solution was poured onto the potential
mdp-2-p/isosafrole. Nothing happen. It was mixed, swirled, shaken.
Nothing happened. The chemist felt at this point that the reaction
had failed, and moved onto other things.

Then the chemist read TSII again, and saw Strike's amazingly
fucking salient advice to add some ethanol. Approx. the
same vol of ethanol to the oil, and immediantly a huge mess of
crystals formed, beyond their wildest expectations. Woo-hoo!