反应详情

温度

180 °C

A mixture of 4-chloro-5-fluoro-1H-pyrrolo[2,3-b]pyridine (30 mg) and piperidine (50 mg) in 1-butanol (0.4 mL) was heated in the microwave reactor (120° C., 0.5 hour, 180° C., 2 hours). The reaction mixture was allowed to cool to ambient temperature and diluted with EtOAc (10 mL) and half-saturated aqueous sodium hydrogencarbonate (10 mL). The aqueous phase was extracted with EtOAc (10 mL) two times and combined organic layers were washed with brine (20 mL), dried over MgSO4, and concentrated. Purification of the crude product by preparative silica gel thin-layer chromatography (EtOAc) gave 5-fluoro-4-(1-piperidinyl)-1H-pyrrolo[2,3-b]pyridine (10 mg) as a white solid.

1. temperatureto cool to ambient temperature
2. extractionThe aqueous phase was extracted with EtOAc (10 mL) two times
3. washwere washed with brine (20 mL)
4. dry with materialdried over MgSO4
5. concentrationconcentrated
6. customPurification of the crude product by preparative silica gel thin-layer chromatography (EtOAc)