HRID576015

反应详情

EQUATION

反应方程式

HRID 576015 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

In a glass autoclave, 240 g of hexamethylenediamine, 52 g of water, 6.4 g of Raney® nickel (doped with 1.5% by weight of chromium), 0.18 g (4 mmol) of potassium hydroxide, 75.1 g (0.37 mol) of butyl ethyl(2-cyanoethyl)phosphinate (produced as in Example 8) are reacted at 50° C. with hydrogen at 25 bar. After 8 hours, the autoclave is let down. For purification, the reaction solution is filtered, passed through a column charged with Deloxan® THP II and concentrated in vacuo. The product is purified by chromatography to obtain 62.0 g (81% of theory) of butyl ethyl(3-aminopropyl)phosphinate as colorless oil.

WORKUP

后处理

  1. customFor purification
  2. filtrationthe reaction solution is filtered
  3. additioncharged with Deloxan® THP II
  4. concentrationconcentrated in vacuo
  5. customThe product is purified by chromatography