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Benzene → HCID 23081970, 화합물

HRID 2238606
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HRID 2238606 반응식
I[C:2]1[CH:3]=[C:4]([CH:10]=[CH:11][C:12]=1[O:13][CH2:14]/[CH:15]=[CH:16]/[CH2:17][C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1)[C:5]([O:7][CH2:8][CH3:9])=[O:6].CC(N=NC(C#N)(C)C)(C#N)C.C1C=CC=CC=1>>[C:18]1([CH2:17][CH2:16][CH:15]2[C:2]3[CH:3]=[C:4]([C:5]([O:7][CH2:8][CH3:9])=[O:6])[CH:10]=[CH:11][C:12]=3[O:13][CH2:14]2)[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 3

HCID 241BenzeneHCID 6547AzobisisobutyronitrileHCID 57445527HCID 57445527, 화합물

생성물 1

HCID 23081970HCID 23081970, 화합물수율 97.2%

실험 절차

To a solution of ethyl 3-iodo-4-{[(2E)-4-phenyl-but-2-enyl]-oxy}benzoate (13.42 g, 31.73 mmol) and AIBN (0.52 g, 3.17 mmol) in benzene (900 ml) tributyltin hydride (12 ml, 44.43 mol) was added at room temperature and the reaction mixture was warmed to reflux. After 2 h, the solvent was eliminated under vacuum. The residue was purified by flash chromatography on silica gel (petroleum ether/ethyl acetate=95/5) affording 9.14 g of the title compound (97% yield).

후처리

  1. temperaturethe reaction mixture was warmed to reflux
  • customThe residue was purified by flash chromatography on silica gel (petroleum ether/ethyl acetate=95/5)
  • 출처 및 근거

    ORD 기록
    ord-15f04a434045465ba40ee1d6a4f26669
    출처 데이터셋
    uspto-grants-2010_05
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US07718815B2

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