HRID1912021
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customequipped with stirrer
- temperaturereflux condenser
- temperaturethermometer and nitrogen inlet, and heated
- distillationis distilled off in vacuo
- customChromatographic purification