反应详情

温度

200 °C

A mixture of 4-chloro-5-fluoro-1H-pyrrolo[2,3-b]pyridine (30 mg) and cyclohexylamine (87 mg) in DMI (0.4 mL) was heated in the microwave reactor (200° C., 4 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 (2×10 mL) 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 N-cyclohexyl-5-fluoro-1H-pyrrolo[2,3-b]pyridin-4-amine (5 mg) as a yellow solid.

1. temperatureto cool to ambient temperature
2. extractionThe aqueous phase was extracted with EtOAc (2×10 mL)
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)