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

HRID 622871

반응식

HRID 622871 반응식
[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]

참가 물질

6

반응물 3

HCID 222AmmoniaHCID 10037677Ethyl 2-cyanoethyl(diethoxymethyl)phosphinateHCID 178418361HCID 178418361, 화합물

생성물 1

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

시약·촉매·용매 2

HCID 935Nickel촉매HCID 702Ethanol용매2회

실험 절차

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).

후처리

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

출처 및 근거

ORD 기록
ord-bc49e0c07875496fa1160739d5ee5c2f
출처 데이터셋
uspto-grants-1988_09
특허 번호
US04772738

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