反应详情

温度

100 °C

A mixture of Example 236A (2 g, 6.29 mmol), (5-fluoro-2-methoxyphenyl)boronic acid (1.284 g, 7.55 mmol), sodium hydrogencarbonate (1.586 g, 18.88 mmol) and [1,1′-bis(diphenylphosphino)ferrocene]-dichloropalladium(II)-dichloromethane adduct (0.276 g, 0.378 mmol) in 80 mL N,N-dimethylformamide and 20 mL water was degassed with nitrogen and heated at 100° C. for 3 hours. The mixture was cooled to room temperature, diluted with water, and extracted with ethyl acetate. The organic phase was washed with brine, dried over magnesium sulfate, filtered and concentrated. Purification by silica-gel flash chromatography (AnaLogix IntelliFlash 280) eluting with dichloromethane afforded the title compound. MS (ESI+) m/z 408 (M+H)+.

1. temperatureThe mixture was cooled to room temperature
2. extractionextracted with ethyl acetate
3. washThe organic phase was washed with brine
4. dry with materialdried over magnesium sulfate
5. filtrationfiltered
6. concentrationconcentrated
7. customPurification by silica-gel flash chromatography (AnaLogix IntelliFlash 280)
8. washeluting with dichloromethane