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Hexamethylenediamine → Butyl ethyl-3-hydroxypropylphosphinate

HRID 1911718
ノート
印刷プレビュー

反応式

HRID 1911718 の反応式
NCCCCCCN.[CH2:9]([P:11]([CH2:18][CH2:19][CH:20]=[O:21])(=[O:17])[O:12][CH2:13][CH2:14][CH2:15][CH3:16])[CH3:10].[H][H]>[Ni].[OH-].[K+].O>[CH2:9]([P:11]([CH2:18][CH2:19][CH2:20][OH:21])(=[O:17])[O:12][CH2:13][CH2:14][CH2:15][CH3:16])[CH3:10]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 3

HCID 16402HexamethylenediamineHCID 86656679Butyl ethyl(2-formylethyl)phosphinateHCID 178418361HCID 178418361、化合物

生成物 1

HCID 86656676Butyl ethyl-3-hydroxypropylphosphinate収率 83%

試薬・触媒・溶媒 3

HCID 935Nickel触媒HCID 14797Potassium Hydroxide触媒
HCID 962Water溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-0380eebd071740d2bd2dca1f029adfcf
出典データセット
uspto-grants-2013_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08604108B2

反応ノート

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