HRID1912021

反应详情

EQUATION

反应方程式

HRID 1912021 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

150 g (1 mol) of butyl ethylphosphonite (produced as in Example 2) and 68.4 g (1.2 mol) of allylamine are initially charged in 200 ml of butanol in a four-neck round-bottom flask equipped with stirrer, reflux condenser, thermometer and nitrogen inlet, and heated. At about 100° C., in the course of 1 h, 98.4 g of a 5% solution of AIBN in butanol are added dropwise, whereafter the solvent is distilled off in vacuo. Chromatographic purification yields 135 g (65% of theory) of butyl ethyl(3-aminopropyl)phosphinate.

WORKUP

后处理

  1. customequipped with stirrer
  2. temperaturereflux condenser
  3. temperaturethermometer and nitrogen inlet, and heated
  4. distillationis distilled off in vacuo
  5. customChromatographic purification