Sodium cyanoborohydride → HCID 58443691, compound

Participants

Reaction Steps

To a solution of 4-(2,4,6-trichloro-phenyl)-butan-2-one O-methyl-oxime (0.650 g, 2.33 mmol) in acetic acid, sodiumcyanoborohydride (0.293 g, 4.66 mmol) was added. The reaction mass was stirred at room temp for 6 hours. When the TLC confirmed the completion of the reaction, the acetic acid in the reaction mass was removed by azeotropic distillation. The residue was then basified with 10% NaOH solution and it was extracted with ethyl acetate (3×30 ml). The combined ethyl acetate layers were washed with water followed by brine solution and dried over sodium sulfate before concentration. Resulting crude mass was purified by column chromatography using 60-120μ mesh silica gel and product collected at 3% ethyl acetate in hexane as eluent to give O-Methyl-N-[1-methyl-3-(2,4,6-trichloro-phenyl)-propyl]-hydroxylamine (0.6 g, 90%).

Provenance & Evidence