HRID1077696

反应详情

EQUATION

反应方程式

HRID 1077696 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 1.86 g of 3-(p-chlorobenzylamino)propyl(n-butyl)phosphinic acid ethyl ester in 30 ml of semi-concentrated hydrochloric acid is heated under reflux overnight, a clear solution forming after only 10 minutes. The solution is then cooled to 0°, whereupon a white precipitate forms. The precipitate is filtered off, washed with water and dried under reduced pressure at 60°. Recrystallisation from water and drying yield 3-(p-chlorobenzylamino)propyl(n-butyl)phosphinic acid hydrochloride having a melting pint of 212°-214°.

WORKUP

后处理

  1. temperatureunder reflux overnight
  2. customa clear solution forming after only 10 minutes
  3. temperatureThe solution is then cooled to 0°, whereupon a white precipitate forms
  4. filtrationThe precipitate is filtered off
  5. washwashed with water
  6. customdried under reduced pressure at 60°
  7. customRecrystallisation from water
  8. customdrying