Reaktion #663197

Reaktionsgleichung

hexamethylenediamine

butyl ethyl(2-cyanoethyl)phosphinate

hydrogen

→

butyl ethyl(3-aminopropyl)phosphinate

Ausbeute 81.0%

Lösungsmittel

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeFor purification
2. 2
   Filtrationthe reaction solution is filtered
3. 3
   workup.ADDITIONcharged with Deloxan® THP II
4. 4
   Einengenconcentrated in vacuo
5. 5
   SonstigeThe product is purified by chromatography

Vorschrift

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.

Quelle