反应详情

To a solution of 4-bromo-3-trifluoromethoxy-phenylamine (500 mg, 2 mmol) in DCM (5 mL) was added N,N-carbonyldiimidazole (348 mg, 2.15 mmol). The reaction mixture was stirred at RT overnight and then 4-piperazin-1-yl-piperidine-1-carboxylic acid tert-butyl ester (579 mg, 2.15 mmol, Preparation 12) was added and the reaction mixture was stirred at RT for 15 min, and concentrated by rotary evaporation and purified by silica gel chromatography (80 g silica, 0-10% MeOH/DCM) to provide the title intermediate (776 mg, 70% yield) as a yellow powder. (m/z): [M+H]+ calcd for C22H30BrF3N4O4 551.14, found 551.3.

1. stirringthe reaction mixture was stirred at RT for 15 min
2. concentrationconcentrated by rotary evaporation
3. custompurified by silica gel chromatography (80 g silica, 0-10% MeOH/DCM)