反应详情

温度

35 °C

Method J—Step a To a mixture of 1-[3-(5-Chloro-1H-benzoimidazol-2-yl)-4-fluoro-phenyl]-piperidine-4-carboxylic acid hydrochloride (obtained as described in general method 10, step b) (0.01 g, 0.25 mmol) in dcm (2 mL), HATU (0.10 g, 0.26 mmol), TEA (0.07 mL, 0.55 mmol) and N,N′-dimethyl-3-aminopyrrolidine (0.04 g, 0.31 mmol) were added. The reaction mixture was heated at 35° C. overnight, cooled to room temperature and washed with ammonium chloride solution (2 mL), saturated Na2CO3 solution (2 mL) and water (2 mL). The organic layer was then filtrated on an NH2 cartridge and further purified by flash chromatography (eluent: EtOAc:NH3 2N in MeOH/9:1) to obtain 0.03 g of the title compound (30%).

1. additionwere added
2. temperaturecooled to room temperature
3. washwashed with ammonium chloride solution (2 mL), saturated Na2CO3 solution (2 mL) and water (2 mL)
4. filtrationThe organic layer was then filtrated on an NH2 cartridge
5. customfurther purified by flash chromatography (eluent: EtOAc:NH3 2N in MeOH/9:1)