反应详情

4.85 g (211 mmol) of sodium are dissolved in ethanol (260 ml), 30.0 g (141 mmol) of 3-amino-3-(2,4-dichlorophenyl)acrylonitrile and 36.59 g (310 mmol) of diethyl carbonate are added, and the reaction solution is stirred under reflux for 4 h. Ethyl acetate and water are added to the reaction mixture, and the pH is adjusted to pH=5 with concentrated hydrochloric acid. The organic phase is separated off, dried over magnesium sulphate and concentrated in a rotary evaporator. The residue is chromatographed on silica gel (mobile phase cyclohexane/ethyl acetate 7:1 to 1:1); the product has Rf=0.5 in cyclohexane/ethyl acetate 1:1. 17.1 g (43% of theory) of the product are obtained.

1. temperatureunder reflux for 4 h
2. customThe organic phase is separated off
3. dry with materialdried over magnesium sulphate
4. concentrationconcentrated in a rotary evaporator
5. customThe residue is chromatographed on silica gel (mobile phase cyclohexane/ethyl acetate 7:1 to 1:1)
6. custom17.1 g (43% of theory) of the product are obtained