反应详情

To a stirred solution of crude 1-(2,4,6-trichloro-phenyl)-propan-2-one O-methyl-oxime prepared as described in example P4, (12.3 g, 0.046 mol) in acetic acid (120 ml), sodium cyanoborohydride (6.1 g, 0.097 mol) was added portionwise at 12 to 15° C. The reaction mass was stirred at ambient temperature for 18 hours. TLC confirmed the completion of reaction, then solvent was evaporated under reduced pressure (co-evaporation with toluene twice). The resulting residue was poured on to 1 N sodium hydroxide solution (150 ml) and extracted with dichloromethane (2×100 ml). The combined organic layer was washed with water (2×100 ml) followed by drying over anhydrous sodium sulfate before evaporating the solvent to afford crude O-Methyl-N-[1-methyl-2-(2,4,6-trichloro-phenyl)-ethyl]-hydroxylamine (12.3 g, 100%).

1. customthe completion of reaction
2. customsolvent was evaporated under reduced pressure (co-evaporation with toluene twice)
3. additionThe resulting residue was poured on to 1 N sodium hydroxide solution (150 ml)
4. extractionextracted with dichloromethane (2×100 ml)
5. washThe combined organic layer was washed with water (2×100 ml)
6. dry with materialby drying over anhydrous sodium sulfate
7. custombefore evaporating the solvent