反应详情

To a solution of 5.7 g (0.0224 mol) of isopropyl 3-aminopropyl(benzyl)phosphinate in 50 ml of chloroform 9.91 ml (0.0922 mol) of trimethylsilylbromide are added raising the temperature to 44°. The reaction mixture is stirred at 50° for 4 hours and then at room temperature overnight. Removal of the chloroform and excess trimethylsilylbromide under reduced pressure yields an oil which is taken up in isopropanol and 20 ml of propylene oxide. After stirring for 10 minutes, a white solid precipitates. The solid is filtered off and dried over phosphorous pentoxide yielding 3-aminopropyl(benzyl)phosphinic acid, m.p. 278-280°.

1. temperatureraising the temperature to 44°
2. customat room temperature
3. customovernight
4. customRemoval of the chloroform and excess trimethylsilylbromide under reduced pressure
5. customyields an oil which
6. stirringAfter stirring for 10 minutes
7. customa white solid precipitates
8. filtrationThe solid is filtered off
9. dry with materialdried over phosphorous pentoxide