反应详情

15.0 g of n-butylphosphinic acid ethyl ester and 5.3 g of acrylonitrile are dissolved under argon in 25 ml of ethanol. The solution is cooled to 10°, and a solution of 1.15 g of sodium in 50 ml of ethanol is added dropwise, whereupon an exothermic reaction takes place. The mixture is then heated under reflux for one hour and cooled to room temperature, and 3.3 g of glacial acetic acid are added. The solvent is removed and the residue is taken up in dichloromethane. The resulting solution is washed with water, dried over sodium sulfate and concentrated by evaporation. The oil that remains is distilled, yielding 2-cyanoethyl(n-butyl)phosphinic acid ethyl ester having a boiling point of 120° (10-1 bar).

1. temperatureThe solution is cooled to 10°
2. temperatureThe mixture is then heated
3. temperatureunder reflux for one hour
4. customThe solvent is removed
5. washThe resulting solution is washed with water
6. dry with materialdried over sodium sulfate
7. concentrationconcentrated by evaporation
8. distillationThe oil that remains is distilled