HRID1612668

反应详情

EQUATION

反应方程式

HRID 1612668 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of 6.7 g of 3-(benzyloxycarbonylamino)propyl(n-butyl)phosphinic acid in 125 ml of 36% hydrochloric acid is heated at reflux for 1.5 hour. The mixture is evaporated to an oil and the oil is co-evaporated with water (2×50 ml) to give a white solid. This solid is then dissolved in 50 ml of dry methanol, 1-3 ml of propylene oxide is added and the solution is stirred at room temperature. The precipitated product is collected by filtration and dried to give 3-aminopropyl(n-butyl)phosphinic acid, m.p. 231°-234° (dec.), 31P-NMR: δ=+44.6 ppm (D2O).

WORKUP

后处理

  1. temperatureat reflux for 1.5 hour
  2. customThe mixture is evaporated to an oil
  3. customto give a white solid
  4. filtrationThe precipitated product is collected by filtration
  5. customdried