HCID 86657769, compound → HCID 58443674, compound

Participants

Reaction Steps

To a stirred solution of 3-(2,4,6-trichloro-phenyl)-propionaldehyde O-methyl-oxime in acetic acid, NaCNBH3 was added at 0° C.-10° C. The reaction mass was then stirred at ambient temperature for 6 hours. When the TLC confirmed completion of the reaction, acetic acid was removed by azeotropic distillation. The residue was basified with 10% NaOH solution and aqueous solution was extracted with ethyl acetate (3×30 ml). The combined organic layer was washed with water and brine. The organic layer was then dried over anhydrous sodium sulphate and concentrated under reduced pressure. The resulting crude mass was purified over column chromatography (silica gel 60-120 mesh, 3% ethyl acetate in hexane) to afford O-methyl-N-[3-(2,4,6-trichloro-phenyl)-propyl]-hydroxylamine (0.4 g, 88%).

Provenance & Evidence