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

HRID 5166노트

반응식

HRID 5166 반응식
[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]

참가 물질

6

반응물 3

HCID 222AmmoniaHCID 14362805Ethyl 1-methyl-2-cyanoethyl(diethoxymethyl)phosphinateHCID 178418361HCID 178418361, 화합물

생성물 1

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

시약·촉매·용매 2

HCID 935Nickel촉매HCID 702Ethanol용매2회

실험 절차

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).

후처리

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

출처 및 근거

ORD 기록
ord-8451bd41350741798488ec1da4264c87
출처 데이터셋
uspto-grants-1993_09
특허 번호
US05243062

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