Cyclohexene, 4,4-difluoro-1-[(trimethylsilyl)oxy]- → 4,4-Difluorocyclohex-2-en-1-one

HRID 337855노트

반응식

HRID 337855 반응식
[F:1][C:2]1([F:13])[CH2:7][CH2:6][C:5]([O:8][Si](C)(C)C)=[CH:4][CH2:3]1>C(#N)C.C([O-])(=O)C.[Pd+2].C([O-])(=O)C>[F:1][C:2]1([F:13])[CH2:7][CH2:6][C:5](=[O:8])[CH:4]=[CH:3]1

참가 물질

4

반응물 1

HCID 89962723Cyclohexene, 4,4-difluoro-1-[(trimethylsilyl)oxy]-

생성물 1

HCID 899621164,4-Difluorocyclohex-2-en-1-one수율 50.5%

시약·촉매·용매 2

HCID 167845palladium(II) acetate촉매HCID 6342Acetonitrile용매

실험 절차

To a solution of the [(4,4-difluorocyclohex-1-en-1-yl)oxy](trimethyl)silane (3.1 g, 15.0 mmol) prepared in Example 88a in acetonitrile (25 mL), palladium acetate (4.0 g, 17.8 mmol) was added, and the mixture was stirred at room temperature for 45 minutes. The reaction solution was filtered, the filtrate was vacuum concentrated, and the residue was purified with silica gel chromatography (hexane/ethyl acetate=9:1) to yield the title compound (1.0 g, 50%) as a yellow oil.

후처리

  1. filtrationThe reaction solution was filtered
  2. concentrationconcentrated
  3. customthe residue was purified with silica gel chromatography (hexane/ethyl acetate=9:1)

출처 및 근거

ORD 기록
ord-98f4e68716674df2b71a84d4f7468771
출처 데이터셋
uspto-grants-2014_11
특허 번호
US08889741B2

반응 노트

불러오는 중…