反应详情

4.85 g (211 mmol) of sodium were 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 were added and the reaction solution was stirred under reflux for 4 h. Ethyl acetate and water were added to the reaction mixture, and the pH was adjusted to pH=5 with concentrated hydrochloric acid. The organic phase was separated off, dried over magnesium sulfate and concentrated on a rotary evaporator. The residue was chromatographed on silica gel (mobile phase cyclohexane/ethyl acetate 7:1 to 1:1), the product had an Rf=0.5 in cyclohexane/ethyl acetate 1:1. This gave 17.1 g (43% of theory) of the product.

1. temperatureunder reflux for 4 h
2. customThe organic phase was separated off
3. dry with materialdried over magnesium sulfate
4. concentrationconcentrated on a rotary evaporator
5. customThe residue was chromatographed on silica gel (mobile phase cyclohexane/ethyl acetate 7:1 to 1:1)