Ammonia → Ethyl 3-amino-1-methylpropyl(diethoxymethyl)phosphinate

HRID 542294ノート

反応式

HRID 542294 の反応式
[CH3:1][CH:2]([P:6]([CH:11]([O:15][CH2:16][CH3:17])[O:12][CH2:13][CH3:14])(=[O:10])[O:7][CH2:8][CH3:9])[CH2:3][C:4]#[N:5].N.[H][H]>C(O)C.[Ni]>[NH2:5][CH2:4][CH2:3][CH:2]([P:6]([CH:11]([O:15][CH2:16][CH3:17])[O:12][CH2:13][CH3:14])(=[O:10])[O:7][CH2:8][CH3:9])[CH3:1]

参加物

6

反応物 3

HCID 222AmmoniaHCID 14362805Ethyl 1-methyl-2-cyanoethyl(diethoxymethyl)phosphinateHCID 178418361HCID 178418361、化合物

生成物 1

HCID 14362808Ethyl 3-amino-1-methylpropyl(diethoxymethyl)phosphinate

試薬・触媒・溶媒 2

HCID 935Nickel触媒HCID 702Ethanol溶媒2 回

実験手順

A solution of 17.0 g of ethyl 1-methyl-2-cyanoethyl(diethoxymethyl)phosphinate in 150 ml of ethanol is added to 155.0 g of an 8% solution of ammonia in ethanol. To this are added 10 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 and the filtrate is concentrated under reduced pressure and the crude product is distilled under reduced pressure to give ethyl 3-amino-1-methylpropyl(diethoxymethyl)phosphinate, b.p. 140° C./0.01 mbar, 31P=+47.0 and +46.7 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 under reduced pressure

出典と根拠

ORDレコード
ord-38590387869242bd8ea74cdcf20cd947
出典データセット
uspto-grants-1987_04
特許番号
US04656298

反応ノート

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