反应详情

3-Trifluoromethylphenyl thiourea (3.00 g, 13.6 mmol), 4-cyanobenzaldehyde (3.57 g, 27.3 mmol) and ethyl acetoacetate (3.55 g, 27.3 mmol) are dissolved in 50 ml THF. Ethyl polyphosphate (4.50 g) is added and the reaction mixture is stirred at reflux temperature overnight. After cooling to room temperature, it is quenched with 50 ml of water and extracted with 100 ml ethyl acetate (2×). The combined organic layers are dried with sodium sulfate and the solvent is removed in vacua. The product is purified via preparative HPLC (RP18-column; eluent: acetonitrile-water, gradient 10:90 to 90:10).

1. temperatureat reflux temperature overnight
2. customit is quenched with 50 ml of water
3. extractionextracted with 100 ml ethyl acetate (2×)
4. dry with materialThe combined organic layers are dried with sodium sulfate
5. customthe solvent is removed in vacua
6. customThe product is purified via preparative HPLC (RP18-column; eluent: acetonitrile-water, gradient 10:90 to 90:10)