Ethyl 3-amino-2-phenylpropyl(diethoxymethyl)phosphinate → Ethyl 3-amino-2-cyclohexylpropyl(diethoxymethyl)phosphinate

HRID 542310

반응식

HRID 542310 반응식
[NH2:1][CH2:2][CH:3]([C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1)[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]>C(O)(C)(C)C.[Rh]>[NH2:1][CH2:2][CH:3]([CH:17]1[CH2:18][CH2:19][CH2:20][CH2:21][CH2:22]1)[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

4

반응물 1

HCID 14362832Ethyl 3-amino-2-phenylpropyl(diethoxymethyl)phosphinate

생성물 1

HCID 19379613Ethyl 3-amino-2-cyclohexylpropyl(diethoxymethyl)phosphinate

시약·촉매·용매 2

HCID 23948Rhodium촉매HCID 6386tert-Butanol용매2회

실험 절차

A solution of 3.45 g of ethyl 3-amino-2-phenylpropyl(diethoxymethyl)phosphinate in 25 ml of tertiary butanol is added to 2.0 g of 5% rhodium in alumina, suspended in 25 ml of tertiary butanol. The resulting mixture is hydrogenated at an atmosphere of 150 bar and temperature of 100° C. for a period of 20 hours. The mixture is then filtered and the filtrate is concentrated under reduced pressure. The crude product is chromatographed on silica gel using ethanol as eluent to give ethyl 3-amino-2-cyclohexylpropyl(diethoxymethyl)phosphinate as a viscous oil, 31P=47.1 and +47.0 ppm (CDCl3).

후처리

  1. filtrationThe mixture is then filtered
  2. concentrationthe filtrate is concentrated under reduced pressure
  3. customThe crude product is chromatographed on silica gel

출처 및 근거

ORD 기록
ord-dc54921fbaa9426999a526b42a837206
출처 데이터셋
uspto-grants-1987_04
특허 번호
US04656298

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