Hi!
Swim made 5.5 g of crude nitroethane ala Antoncho and immediately proceeded with the 2,5-DMBA condensation to form the nitropropene. Swim did this, as described in pihkal and used acetic acid as solvent and ammoniumacetate as catalyst. The color shift proceeded excactly like swim has previously seen in the 2,5-DMBA + Nitromethane to form the nitrostyrene synth, so swim suspects that the nitroethane was just dandy.
When the reaction had refluxed for three hours, the heat was removed and the color was noted to be very dark red/black and gave yellow "stains" that slowly ran down the side of the glass, when shaken in the flask(corresponds 100% to the nitrostyrene synth). The solvent was removed at atm pressure, and swim thought, that he would be a wise bee and simply recrystallize right away as done in the nitrostyrene synth, so swim added some IPA and shaked the mixture. This was placed in the fridge and a couple of hours later it was taken out. Alas no crystals had formed
Swim suspects that the nitropropene was TO crude, to be recrystallized and Shulgin yet again was right and one actually have to wash the reaction mixture at first. Swim was thinking of this scheme to save his precious nitropropene:
Distill of the IPA and suspend residue in water.
Extract the water/nitropropane/gunk mixture with methylene chloride(no chloroform avavible) three times and evaporate the solvent and THEN recrystallize.
Any ideas on how to save swims dream? Is methylenechloride ok for extraction or do you have better suggestions?
Thank you so much for you help!
Regards
Peter