posted 10-31-1999 07:40 PM
I have this data imprinted in my cerebral cortext but there is one detail
that is required.
How much DCM was used in the final extraction??
Isosafrole > MDP2P Via Modified Performic Acid
Combine 16.25 grams of Isosafrole with 50 ml DCE (Dichloroethane) or
[DCM] plus 5 Grams Sodium bicarbonate (Sodium Hydrogen Carbonate), let it
stirr for 3 hours.
Slowly combine 25 grams 86% Formic acid and 15.1 grams 38% Hydrogen
Peroxide (to create Performic acid) and cool to 0 C.
*Then drip the Performic acid VERY VERY slowly , into the ISO-DCE-SBC
mix, keeping temp under 40 C until in, and stir vigerously for 10 hours.
Stop stirring and let it sit for one hour in seperatory funnel.It will
be orange juice color on top and clearish peracid mix on bottom, seperate
into new FBF (orange layer) .Evaporate (no vacuum) off the DCE and stock
it for future use.
Add 180 grams of 15% Sulfuric acid (H2SO4), boil it to reflux with
slight addition of Methanol (60ml) and condenser added for 2 hrs.
Let it cool and extract with DCM, boil off solvent for brown oil that
is peppery and cardamon smell.
Around 16 grams MDP2P.
Thanks Inadvance
Regards
Synthia