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HCID 15735543, 화합물 → HCID 15735657, 화합물

HRID 704608
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HRID 704608 반응식
[CH:1]1(/[CH:7]=[C:8](\[CH2:14][P:15]([O:21]CC)([CH2:17][CH:18]([CH3:20])[CH3:19])=[O:16])/[C:9]([O:11][CH2:12][CH3:13])=[O:10])[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.C(Cl)(Cl)Cl.CO.C(O)(=O)C>Cl.C(OCCCC)(=O)C>[CH:1]1(/[CH:7]=[C:8](\[CH2:14][P:15]([OH:21])([CH2:17][CH:18]([CH3:20])[CH3:19])=[O:16])/[C:9]([O:11][CH2:12][CH3:13])=[O:10])[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 15735543HCID 15735543, 화합물HCID 21866353chloroform methanol HOAc

생성물 1

HCID 15735657HCID 15735657, 화합물수율 94%

시약·촉매·용매 1

HCID 20072624HCID 20072624, 화합물용매

실험 절차

A solution of 107 mg (0.31 millimole) of ethyl (Z)-3-cyclohexyl-2-(ethoxyisobutylphosphinoyl)methylpropenoate in 1.0 ml of 4N HCl-butyl acetate was heated in a sealed tube at 100° C for 2 hours. After cooling, the solvent was evaporated under reduced pressure, and the residue was purified by "dry-column" flash chromatography 15 g of silica gel 60 made by E. Merck & Co.; chloroform-methanol-acetic acid (50:1:1)] to give 91 mg (yield 94%) of the captioned compound as a colorless oil.

후처리

  1. temperatureAfter cooling
  2. customthe solvent was evaporated under reduced pressure
  3. customthe residue was purified by "dry-column" flash chromatography 15 g of silica gel 60

출처 및 근거

ORD 기록
ord-6730d607e7f34f129051f00d74dbd838
출처 데이터셋
uspto-grants-1991_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04988681

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