反应详情

To an emulsion of diethyl 3-bromo-2,4,5-trifluorobenzoylmalonate (3.25 g) in water (4 ml) was added p-toluenesulfonic acid (4 mg) and refluxed for 3 hours with vigorous stirring. After cooling, the reaction mixture was extracted with dichloromethane (8 ml×4). The organic layer was washed with water saturated with sodium chloride, dried over anhydrous sodium sulfate and concentrated. The residue was recrystallized from dichloromethane-n-hexane to give the title compound (1.51 g), mp 85°-88° C.

1. temperaturerefluxed for 3 hours with vigorous stirring
2. temperatureAfter cooling
3. extractionthe reaction mixture was extracted with dichloromethane (8 ml×4)
4. washThe organic layer was washed with water saturated with sodium chloride
5. dry with materialdried over anhydrous sodium sulfate
6. concentrationconcentrated
7. customThe residue was recrystallized from dichloromethane-n-hexane