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Tetrafluoroborate → Ethyl-4,4-difluorocyclohexane carboxylate

HRID 1193001
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HRID 1193001 반응식
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]
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참가 물질

5

반응물 3

HCID 26255TetrafluoroborateHCID 317638Ethyl 4-oxocyclohexanecarboxylateHCID 10891295Tetrabutylammonium bifluoride

생성물 1

HCID 2779138Ethyl-4,4-difluorocyclohexane carboxylate수율 68%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-70ec3e09b81344e8b727ff26f4b030ca
출처 데이터셋
uspto-grants-2014_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08680332B2

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