From J.of Analytical Toxicology vol.6 p.71-75 (1986).By A.T.Shulgin et al., A soln. of piperonal 15 g. in 80 ml. acetic acid was treated with 15 ml. nitroethane and 7 g. anhydrous ammonium acetate, and heated at 100 degrees for 4 hrs. The addition of a few ml. water followed by cooling yielded 8.0 g. 1-(3,4-methylenedioxyphenyl)-2-nitropropene, m.p.97-98 degrees. Recrystallized from acetic acid. This product was dissolved in boiling acetic acid, and added to a suspension of elemental iron (18.0 g. electrolytic grade) in 100 ml. warm acetic acid. The mixture was heated gently, with frequent swirling, until an exothermic reaction ensued. After the reaction had subsided, one liter of water added, and the mixture clarified by filtration. The filtrate was extracted with 75 ml. methylene chloride three times, the extracts pooled, washed once with 5% sodium hydroxide, and the solvent removed in vacuum. Distillation of the residue yielded 4.6 g. 3,4-methylenedioxyphenylacetone as a colourless oil. b.p. 100-110 degrees at 0.2 mm/mercury.
Chemical supply houses sell inacurate chemicals in place of this compound.
