反应详情

To an emulsion of diethyl 2-(3-bromo-2-chloro-4,5-difluorobenzoyl)malonate (11.44 g) in water (16 ml) was added p-toluenesulfonic acid (15 mg) and refluxed for 3 hours with stirring vigorously. After cooling, the reaction mixture was extracted with dichloromethane. The organic layer was washed with water, dried over anhydrous sodium sulfate and concentrated. The residue was purified by silica gel chromatography eluting with dichloromethane-n-hexane (1:1) to give the title compound (4.56 g), mp 47°-51° C.

1. temperaturerefluxed for 3 hours
2. temperatureAfter cooling
3. extractionthe reaction mixture was extracted with dichloromethane
4. washThe organic layer was washed with water
5. dry with materialdried over anhydrous sodium sulfate
6. concentrationconcentrated
7. customThe residue was purified by silica gel chromatography
8. washeluting with dichloromethane-n-hexane (1:1)