反应详情

温度

0 °C

At 0° C., 200 mg (0.55 mmol) of N-{5-[4-(trifluoromethoxy)phenyl]piperidin-3-yl}benzamide and 153 μl (1 l mmol) of triethylamine were initially charged in 17 ml of dichloromethane, and 111 mg (0.55 mmol) of 4-nitrophenyl chlorocarbonate were added slowly. The mixture was stirred at 0° C. for 2 h and then warmed to RT. Water and saturated aqueous sodium bicarbonate solution were added, and the reaction mixture was extracted. The organic phase was dried over sodium sulphate and concentrated under reduced pressure. The crude product was then purified by preparative HPLC (Reprosil C18, water/acetonitrile gradient). Yield: 254 mg (87% of theory)

1. temperaturewarmed to RT
2. extractionthe reaction mixture was extracted
3. dry with materialThe organic phase was dried over sodium sulphate
4. concentrationconcentrated under reduced pressure
5. customThe crude product was then purified by preparative HPLC (Reprosil C18, water/acetonitrile gradient)