HRID1911718

反应详情

EQUATION

反应方程式

HRID 1911718 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-formylethyl)phosphinate (produced in as Example 9) are reacted at 50° C. with hydrogen at 25 bar. Following a reaction time of 8 hours, the autoclave was 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 63.9 g (83% of theory) of butyl ethyl(3-hydroxypropyl)phosphinate as colorless oil.

WORKUP

后处理

  1. customa reaction time of 8 hours
  2. customFor purification
  3. filtrationthe reaction solution is filtered
  4. additioncharged with Deloxan® THP II
  5. concentrationconcentrated in vacuo
  6. customThe product is purified by chromatography