Hi everyone, this is Dr Gonzo, I am making one of my twice-yearly appearances and after this post I'm afraid I have to go away again.
I have a couple updates regarding Methyl Man's amalgam and my photo essay that appears on Rhodium's page. First, as my client got better with this technique (and double-distilled the ketone), he brought his yields up to 21.0 g of the hydrochloride from 25.0 g of ketone. He maintains his opinion that for the MDMA-producing hobbyist (as opposed to the professional cook) the slightly less-than-perfect yield of the nitromethane Al/Hg is easily offset by the simplicity of the reaction, the unwatched reagents needed, and the good chance of success.
Also, my client asked a friend to do an NMR of some MDMA HCl he had produced with this method. The workup for this batch was a xylene extraction from the reaction mixture, double bicarbonate wash, double NaCl wash, double water wash, dry the approx. 800 mL xylene extraction with MgSO4, then carefully gas, filtering out precipitated crystals often and continuing to gas. Then a final xylene wash of the filtered crystals. Friend was extremely impressed with the purity and estimated it at being 99.5% or better. Any impurities were tiny, tiny peaks on the NMR spectrum, almost not there at all.
I'll probably email Rhodium and ask him to update the essay, and I'll see if I can get the NMR spectrum added too. Keep up the great work, everyone!