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Tetrafluoroborate → Ethyl-4,4-difluorocyclohexane carboxylate

HRID 1193001
ノート
印刷プレビュー

反応式

HRID 1193001 の反応式
F[B-](F)(F)F.CCCC[N+](CCCC)(CCCC)CCCC.[FH:23].[F-:24].[C:25]([CH:30]1[CH2:35][CH2:34][C:33](=O)[CH2:32][CH2:31]1)([O:27][CH2:28][CH3:29])=[O:26]>ClCCl>[C:25]([CH:30]1[CH2:35][CH2:34][C:33]([F:24])([F:23])[CH2:32][CH2:31]1)([O:27][CH2:28][CH3:29])=[O:26]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 26255TetrafluoroborateHCID 317638Ethyl 4-oxocyclohexanecarboxylateHCID 10891295Tetrabutylammonium bifluoride

生成物 1

HCID 2779138Ethyl-4,4-difluorocyclohexane carboxylate収率 68%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To an ice-cold suspension of diethylaminodifluorosulfinium tetrafluoroborate (458 mg, 2.0 mmol) and tetrabutylammonium hydrogen difluoride (463 mg, 2.0 mmol) in dichloromethane (3.0 mL) under nitrogen is added 4-carboethoxycyclohexanone (159 μl, 1.0 mmol). The reaction mixture is allowed to warm to room temperature and stirred for 4 h. The reaction mixture is quenched at room temperature with a saturated aqueous ammonium chloride solution, stirred for 15 min, and the resulting mixture is extracted twice using dichloromethane. The organic phases are combined, dried over magnesium sulfate, filtered and concentrated. The crude product is passed through a pad of silica gel using pentane to provide 1-carboethoxy-4,4-difluorocyclohexane (130 mg, 68%) as a clear oil.

後処理

  1. customThe reaction mixture is quenched at room temperature with a saturated aqueous ammonium chloride solution
  2. stirringstirred for 15 min
  3. extractionthe resulting mixture is extracted twice using dichloromethane
  4. dry with materialdried over magnesium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated

出典と根拠

ORDレコード
ord-70ec3e09b81344e8b727ff26f4b030ca
出典データセット
uspto-grants-2014_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08680332B2

反応ノート

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