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Synthesis of MDE Using Nitroethane

by MaDMAx
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Procedure

10 g of Reynold's Heavy duty aluminum foil were torn up and ground up and placed in a 1 liter, 3 neck, RBF. 300 ml of MeOH with a pinch of mercuric thiocyanate were added [Any mercuric salt can be used] and stirring was commenced.

Into an addition funnel was placed 10 g of yummy yellow MDP-2-P, 10 ml of nitroethane which was purchased from a performance fuel shop, yes, I said nitroethane was found OTC, and it really is nitroethane with a boiling point of 114C, with no engine oil or any crap in it, and a gallon was only a little over $30, and 30 ml methanol.

Once amalgamation had taken place, the ketone/EtNO2 was started dripping at about 2 drips per second until the reaction was going violently. Then drip speed was controlled to keep the reaction going violently, but not out of control. About 15 min were required for the addition. Heat was applied to maintain a reflux while dinner was eaten. About an hour and a half later, the flask was allowed to cool to room temp and 300 ml of 35% NaOH that had been chilled to close to 0C was added. Then the dark grey/almost black solution was extracted 4 times with toluene.

The toluene extractions were combined, washed 4 times with water and once with brine. A few chunks of baked epsom salts were added to the toluene and it was put in the freezer for awhile. The dreaded HCl gassing apparatus was assembled, the toluene decanted from the epsom salts, and bubbled with dry HCl gas. Precipitate was filtered and toluene gassed some more and more precipitate was filtered, then toluene was gassed again and there was no more precipitate. Precipitate was washed with ice cold anhydrous acetone and air dried. Weight was 8.8 g.

Recrystallization was attempted with 63 ml of acetonitrile, which would have worked beautifully with MDMA, but almost none of the MDEA would dissolve even when boiling. another 63 ml was added and brought to boiling, but still most of the powder remained undissolved. Acetonitrile was cooled and MDEA filtered. Acetonitrile was rotovapped leaving behind a residue of MDEA in the flask. Recrystallization was attempted again with isopropyl alcohol. 350 ml of boiling IPA still hadn't dissolved all of the MDEA so a couple of drops of water were added and boiled for a few more minutes until all of the MDEA had dissolved. Some IPA was boiled off, then the beaker was covered with plastic wrap and placed in the freezer. The yield after recrystallization was 7.7 g.