反应详情

温度

80 °C

A mixture of 2-bromo-5-hydroxypyridine (1.2 g, 6.9 mmol), sodium chlorodifluoroacetate (2.1 g, 13.8 mmol), and potassium carbonate (1.24 g, 8.97 mmol) in anhydrous DMF (10 ml) was stirred at 80° C. for 20 h. After cooling to room temperature, the reaction mixture was partitioned between EtOAc and water. The aqueous layer was back extracted with EtOAc and the combined organics was dried (Na2SO4) and concentrated. The crude material was purified by chromatography through a Redi-Sep pre-packed silica gel column (40 g), eluting with a gradient of 0% to 10% EtOAc in hexane, to provide 2-bromo-5-(difluoromethoxy)pyridine (0.89 g, 4.0 mmol, 58% yield) as colorless oil. ESI (M+1) 225.8.

1. temperatureAfter cooling to room temperature
2. customthe reaction mixture was partitioned between EtOAc and water
3. extractionThe aqueous layer was back extracted with EtOAc
4. dry with materialthe combined organics was dried (Na2SO4)
5. concentrationconcentrated
6. customThe crude material was purified by chromatography through a Redi-Sep pre-packed silica gel column (40 g)
7. washeluting with a gradient of 0% to 10% EtOAc in hexane