Ammonia → Phosphinic acid, (3-aminopropyl)(diethoxymethyl)-, ethyl ester

HRID 622871ノート

反応式

HRID 622871 の反応式
[C:1]([CH2:3][CH2:4][P:5]([CH:10]([O:14][CH2:15][CH3:16])[O:11][CH2:12][CH3:13])(=[O:9])[O:6][CH2:7][CH3:8])#[N:2].N.[H][H]>C(O)C.[Ni]>[NH2:2][CH2:1][CH2:3][CH2:4][P:5]([CH:10]([O:14][CH2:15][CH3:16])[O:11][CH2:12][CH3:13])(=[O:9])[O:6][CH2:7][CH3:8]

参加物

6

反応物 3

HCID 222AmmoniaHCID 10037677Ethyl 2-cyanoethyl(diethoxymethyl)phosphinateHCID 178418361HCID 178418361、化合物

生成物 1

HCID 10422382Phosphinic acid, (3-aminopropyl)(diethoxymethyl)-, ethyl ester

試薬・触媒・溶媒 2

HCID 935Nickel触媒HCID 702Ethanol溶媒2 回

実験手順

A solution of 9.6 g of ethyl 2-cyanoethyl(diethoxymethyl)phosphinate in 450 ml of ethanol is added to 82 g of an 8% solution of ammonia in ethanol. To this is added 5 ml of Raney Nickel and the resulting mixture is hydrogenated at 1 bar until the theoretical amount of hydrogen has been taken up. The mixture is then filtered, the filtrate is concentrated under reduced pressure and the crude product is distilled to give ethyl 3-aminopropyl(diethoxymethyl)phosphinate, b.p. 150° C./0.01 mbar, 31P=+46.4 ppm (CDCl3).

後処理

  1. filtrationThe mixture is then filtered
  2. concentrationthe filtrate is concentrated under reduced pressure
  3. distillationthe crude product is distilled

出典と根拠

ORDレコード
ord-bc49e0c07875496fa1160739d5ee5c2f
出典データセット
uspto-grants-1988_09
特許番号
US04772738

反応ノート

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