Triacetoxyperiodinane → 4-(Trifluoromethyl)cyclohexanone

HRID 1361290

反応式

HRID 1361290 の反応式
[F:1][C:2]([F:11])([F:10])[CH:3]1[CH2:8][CH2:7][CH:6]([OH:9])[CH2:5][CH2:4]1.CC(OI1(OC(C)=O)(OC(C)=O)OC(=O)C2C=CC=CC1=2)=O>C(Cl)Cl>[F:1][C:2]([F:10])([F:11])[CH:3]1[CH2:8][CH2:7][C:6](=[O:9])[CH2:5][CH2:4]1

参加物

4

反応物 2

HCID 159087TriacetoxyperiodinaneHCID 27797654-(Trifluoromethyl)cyclohexan-1-ol

生成物 1

HCID 27774914-(Trifluoromethyl)cyclohexanone収率 94.7%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of 4-Trifluoromethylcyclohexanol (4.5 g, 26.7 mmol) in DCM (100 ml) was added Dess-Martin periodinane (13.6 g, 32 mmol), and stirred at rt for 2 h. After the reaction finished, the reaction mixture was concentrated in vacuo, sodium thiosulfate aqueous solution and diethylether were added and stirred at rt for 30 min, and extracted with diethylether. The organic layer was dried over MgSO4, concentrated in vacuo at rt to give the title compound (4.2 g, 94.6%).

後処理

  1. concentrationthe reaction mixture was concentrated in vacuo, sodium thiosulfate aqueous solution and diethylether
  2. additionwere added
  3. stirringstirred at rt for 30 min
  4. extractionextracted with diethylether
  5. dry with materialThe organic layer was dried over MgSO4
  6. concentrationconcentrated in vacuo at rt

出典と根拠

ORDレコード
ord-9a2d600bc0624045b5fc87d95f3ff87c
出典データセット
uspto-grants-2011_02
特許番号
US07879852B2

関連ノート

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