反应详情

To a stirred solution of 5-Bromo-1-difluoromethyl-1H-pyridin-2-one (1 g, 4.46 mmol) in 7 ml acetic acid was added bromine (0.24 ml, 4.46 mmol) drop wise at 0° C. and then the reaction mixture was stirred at rt for 12 hrs. Acetic acid was removed under reduced pressure. To this was added ethylacetate and washed with aq NaHCO3 solution. Organic layer was dried over anhy sodium sulphate and concentrated under reduced pressure. It was purified by column chromatography using 5% ethyl acetate in hexane to afford 3,5-Dibromo-1-difluoromethyl-1H-pyridin-2-one (900 mg, 66.5%).

1. customAcetic acid was removed under reduced pressure
2. additionTo this was added ethylacetate
3. washwashed with aq NaHCO3 solution
4. dry with materialOrganic layer was dried over anhy sodium sulphate
5. concentrationconcentrated under reduced pressure
6. customIt was purified by column chromatography