反应详情

温度

70 °C

To a mixture of 3,6-dibromo-2-methylpyridine (2.00 g, 7.97 mmol) and 2,2-difluoroethanol (981 mg, 12.0 mmol) in THF (100 mL) is added potassium tert-butoxide (1.34 g, 12.0 mmol), and the mixture is stirred at 70° C. for 12 hours. After cooling to room temperature, the resulting mixture is poured to water (200 mL). The aqueous layer is extracted with ethyl acetate (200 mL×2). The organic layer is dried over sodium sulfate and concentrated in vacuo. The residue is purified by column chromatography on silica gel eluting with n-hexane/ethyl acetate (8:1) to give 1.94 g (97% yield) of the title compound as colorless oil.

1. temperatureAfter cooling to room temperature
2. extractionThe aqueous layer is extracted with ethyl acetate (200 mL×2)
3. dry with materialThe organic layer is dried over sodium sulfate
4. concentrationconcentrated in vacuo
5. customThe residue is purified by column chromatography on silica gel eluting with n-hexane/ethyl acetate (8:1)