N-(4-bromo-3-chlorophenyl)-N-methylacetamide

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To a solution of 4-bromo-3-chloroacetanilide (10.0 g, 40.2 mmol) in 50 mL THF is added 60% sodium hydride in mineral oil (2.40 g, 60.0 mmol) and the reaction mixture is stirred for 1 h at RT. The reaction mixture is cooled to 0° C., methyliodide (2.49 mL, 40.0 mmol) is added. After 2 h additional methyl iodide (0.25 mL, 4.0 mmol) is added and the reaction mixture is stirred at RT for 10 min. The reaction mixture is quenched with saturated aqueous ammonium chloride, filtered and extracted with diethyl ether. The organic phases are washed with brine, dried over Na2SO4 and evaporated to dryness. Yield: 10.3 g. The reaction mixture is cooled to 0° C. the reaction mixture is stirred at RT for 10 min The reaction mixture is quenched with saturated aqueous ammonium chloride filtered extracted with diethyl ether The organic phases are washed with brine dried over Na2SO4 evaporated to dryness