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
At room temperature, 2.3 g (0.06 mol) of lithium aluminum hydride in 100 ml absolute diethyl ether in a three-neck flask equipped with stirrer, dropping funnel and high-performance condenser are, while continuously stirring, admixed with a solution of 21.7 g (0.1 mol) of butyl ethyl(2-cyano-2-methylethyl)phosphinate (produced similarly to Example 10) in 100 ml of diethyl ether added dropwise at such a rate that there is a moderate boil of the diethyl ether. This is followed by refluxing for 1 hour and admixing of the reaction solution with 1.8 g (0.1 mol) of water, and the insoluble salts are filtered off, the solvent is removed in vacuo and the product is purified by chromatography to obtain 18.8 g (85% of theory) of butyl ethyl(2-methyl-3-aminopropyl)phosphinate as colorless oil.
WORKUP
后处理
- additionadded dropwise at such a rate that there
- temperatureby refluxing for 1 hour
- customthe solvent is removed in vacuo
- customthe product is purified by chromatography