反应详情

A mixture of diethyl 2-(2,4,5-trifluoro-3-methylbenzoyl)malonate (8.10 g) and p-toluenesulfonic acid (9.6 mg) in water (9.6 ml) was refluxed for 3 hours with stirring vigorously. After cooling, the reacting mixture was extracted with dichloromethane. The organic layer was washed with 7% aqueous sodium bicarbonate solution, dried over anhydrous sodium sulfate and then concentrated under reduced pressure. The resulting residue was allowed to stand in a refrigerator for 2 days, the resulting precipitate was collected by filtration and recrystallized from n-hexane to give the title compound (0.51 g) as colorless prisms, mp 38°-39° C.

1. temperaturewas refluxed for 3 hours
2. temperatureAfter cooling
3. extractionthe reacting mixture was extracted with dichloromethane
4. washThe organic layer was washed with 7% aqueous sodium bicarbonate solution
5. dry with materialdried over anhydrous sodium sulfate
6. concentrationconcentrated under reduced pressure
7. filtrationthe resulting precipitate was collected by filtration
8. customrecrystallized from n-hexane