反应详情

45.0 g ethyl polyphosphate are dissolved in 150 ml dioxane, 15.0 g (73.5 mmol) N-[3-(trifluoromethyl)phenyl]urea, 19.3 g (147 mmol) 4-cyanobenzaldehyde and 20.9 g (147 mmol) allyl acetoacetate are added and the mixture is stirred under reflux overnight. Volatiles are evaporated in vacuo, the remainder is dissolved in ethyl acetate and sequentially washed with saturated aqueous sodium hydrogencarbonate, sodium hydrogensulfite and sodium chloride solution. The organic phase is dried over magnesium sulfate, filtered and evaporated to dryness in vacuo. The crude product is purified by column chromatography on silica gel (eluent: cyclohexane/ethyl acetate).

1. temperatureunder reflux overnight
2. customVolatiles are evaporated in vacuo
3. dissolutionthe remainder is dissolved in ethyl acetate
4. washsequentially washed with saturated aqueous sodium hydrogencarbonate, sodium hydrogensulfite and sodium chloride solution
5. dry with materialThe organic phase is dried over magnesium sulfate
6. filtrationfiltered
7. customevaporated to dryness in vacuo
8. customThe crude product is purified by column chromatography on silica gel (eluent: cyclohexane/ethyl acetate)