反应详情

温度

250 °C

To a solution of 4-chloro-1H-pyrrolo[2,3-b]pyridine (50 mg, 0.33 mmol, prepared according to Thibault, C. et al. Org. Lett. 2003, 5, 5023) in NMP (0.5 mL) were added 4-amino-3-fluorophenol (51 mg, 0.40 mmol) and DIEA (0.1 mL, 0.57 mmol). The mixture was heated at 250° C. in a microwave oven for 1 h and then cooled to room temperature. To the mixture was added NaH (10 mg, 0.4 mmol) and the mixture was again heated at 250° C. for 3 h. After cooling, the mixture was diluted with H2O and extracted with EtOAc. The organic layer was washed with H2O, brine, and dried over MgSO4. After filtration and concentration in vacuo, the residue was purified by flash column chromatography (ISCO RediSep® silica gel cartridge) to give the title compound (15 mg, 19%). MS (ESI) m/z 244.1 (M+H)+.

1. temperaturecooled to room temperature
2. temperaturethe mixture was again heated at 250° C. for 3 h
3. temperatureAfter cooling
4. extractionextracted with EtOAc
5. washThe organic layer was washed with H2O, brine
6. dry with materialdried over MgSO4
7. filtrationAfter filtration and concentration in vacuo
8. customthe residue was purified by flash column chromatography (ISCO RediSep® silica gel cartridge)