反应详情

A solution of 4-[(1,3-dimethyl-1H-pyrazol-5-yl)oxy]-3,5-difluorobenzonitrile (i.e. the product of Step A) (1.38 g, 5.5 mmol) in acetonitrile (20 mL) was stirred at ambient temperature, and N-iodosuccinimide (1.35 g, 6.0 mmol) was added in one portion. The reaction mixture was heated at reflux for 2 h, cooled, and then poured into water (40 mL). The resulting mixture was extracted with ethyl acetate (40 mL). The organic phase was washed with water (20 mL) and saturated aqueous NaHCO3 solution (20 mL), dried over MgSO4, and concentrated under reduced pressure to give the title compound as a tan solid (2.1 g).

1. temperatureThe reaction mixture was heated
2. temperatureat reflux for 2 h
3. temperaturecooled
4. extractionThe resulting mixture was extracted with ethyl acetate (40 mL)
5. washThe organic phase was washed with water (20 mL) and saturated aqueous NaHCO3 solution (20 mL)
6. dry with materialdried over MgSO4
7. concentrationconcentrated under reduced pressure