Psychedelia.dk

SYNTHESIS: A solution of 0.12 g mercuric chloride in 180 mL H2O was added to 5 g aluminum foil that had been cut into 1 inch squares, and amalgamation allowed to proceed for 0.5 h. The gray cloudy aqueous phase was decanted, and the resulting aluminum washed with 2x200 mL H2O. After shaking as dry as possible, there was added, in sequence, a solution of 7.6 g methylamine hydrochloride in an equal weight H2O, 23 mL IPA, 18.3 mL 25% NaOH, 6.72 g 1-(3,4-methylenedioxyphenyl)-2-butanone (see under the recipe of J for its preparation), and finally 44 mL additional IPA. The mixture was occasional swirled, and cooled externally as needed to keep the temperature below 50 °C. After the reduction was completed (no metallic aluminum remaining, only gray sludge), it was filtered and the residues washed with MeOH. The combined filtrate and washes were stripped of organic volatiles under vacuum, the residue treated with 100 mL Et2O, and this was extracted with 2x50 mL 3 N HCl. After washing the pooled aqueous extracts with 3x100 mL CH2Cl2, they were made basic with an excess of 25% NaOH and extracted with 5x50 mL CH2Cl2. Drying of these extracts with anhydrous MgSO4 and removal of the solvent gave a residue that was distilled at 88 °C at 0.08 mm/Hg to give a colorless oil that was dissolved in IPA and neutralized with concentrated HCl. The solids that separated were removed by filtration, Et2O washed, and air dried to provide 6.07 g 2-methylamino-1-(3,4-methylenedioxyphenyl)butane hydrochloride (METHYL-J or MBDB) as white crystals with a mp of 156 °C. Anal. (C12H18ClNO2) C,H,N. Reductive amination of the butanone with methylamine hydrochloride in MeOH, employing sodium cyano-borohydride, gave an identical product but in a smaller yield.