4.4.3 Alternative reduction procedure
For those unable or unwilling to construct the admittedly large number of mechanical items described above, there is an alternative reduction procedure that the reader may or may not find more convenient. This reduction, gleaned from Dr. Alexander Shulgin's wonderful book PIKHAL, uses glacial acetic acid instead of muriatic acid to create hydrogen by reacting with catalytic iron. It also cleans up with water and eliminates the steam distillation step used above. The downside is that, as described, it takes a much larger volume of acid to reduce an equivalent amount of nitropropene. It may be possible to reduce the amount of acid required, and I leave it those interested to develop it further.
Place a 1000ml Pyrex beaker into a pan of water and rest this on a hotplate. Add 140ml of glacial acetic acid and 32g of 80-100 mesh catalytic iron. Heat to about 85癈, just below the point where white salts begin to appear, then add 10-15g of 1-phenyl-2-nitropropene crystals dissolved in 75ml of glacial acetic acid. Add slowly, allowing a vigorous reaction free from excessive frothing. Continue heating for 1.5 hours after the addition. The surface will crust up, turn whitish, and climb the walls of the beaker. Remove from heat, mix into 2000ml of clean water. Add enough concentrated lye solution to neutralize the acid, then extract with methylene chloride and distill exactly as above. One can scale this up by using a bucket made from polypropylene (try Chevron Delo 400 oil buckets). These tough buckets will stand up to 100癈 temperatures without deforming. Or one can use a stainless pot either plain or Teflon coated. Glacial acetic acid has a strong vinegar smell which disperses rapidly when heated, making for an odor problem hard to disguise. But since there is no power required, one can do this in the woods somewhere. This procedure was designed by Dr. Shulgin to reduce the nitrostyrene associated with MDMA, so it can be used for both Meth and Ecstasy if one can find a supply of piperonal. The reader will find that most of the procedures described herein apply to the manufacture of both products. This writer has tried this procedure with excellent results, obtaining a 75% yield of a very pure and colorless P2P.