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

HRID 337855ノート

反応式

HRID 337855 の反応式
[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

参加物

4

反応物 1

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

生成物 1

HCID 899621164,4-Difluorocyclohex-2-en-1-one収率 50.5%

試薬・触媒・溶媒 2

HCID 167845palladium(II) acetate触媒HCID 6342Acetonitrile溶媒

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-98f4e68716674df2b71a84d4f7468771
出典データセット
uspto-grants-2014_11
特許番号
US08889741B2

反応ノート

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