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Chlorodifluoromethane → HCID 21852637, 화합물

HRID 1586351
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HRID 1586351 반응식
[OH-].[Na+].[C:3]([C:6]1[CH:11]=[C:10]([CH3:12])[CH:9]=[C:8]([CH3:13])[C:7]=1[OH:14])(=[O:5])[CH3:4].Cl[CH:16]([F:18])[F:17]>S([O-])(O)(=O)=O.C([N+](CCCC)(CCCC)CCCC)CCC.ClCCl>[F:17][CH:16]([F:18])[O:14][C:7]1[C:8]([CH3:13])=[CH:9][C:10]([CH3:12])=[CH:11][C:6]=1[C:3](=[O:5])[CH3:4]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 6372ChlorodifluoromethaneHCID 14798Sodium HydroxideHCID 27585613',5'-Dimethyl-2'-hydroxyacetophenone

생성물 1

HCID 21852637HCID 21852637, 화합물수율 21%

시약·촉매·용매 2

HCID 94433Tetrabutylammonium hydrogen sulfate촉매HCID 6344Dichloromethane
용매

실험 절차

10 ml of a 30% aqueous sodium hydroxide solution and 8.5 g (0.025 mol) of tetrabutylammonium hydrogensulphate are added to a solution of 8.2 g (0.05 mol) of 2-acetyl-4,6-dimethylphenol, obtained above in Example XXX, in dichloromethane. A stream of chlorodifluoromethane is then passed into the reaction mixture for 30 minutes and the latter is then stirred at room temperature for 4 hours. The reaction mixture is then extracted with dichloromethane and the extract is washed with water. After drying the organic phase over MgSO4 and evaporation, the residue obtained is purified by passing through a silica column (dichloromethane) to lead to the production of a liquid: (2-difluoromethoxy-3,5-dimethylphenyl)ethanone: yield 21%.

후처리

  1. extractionThe reaction mixture is then extracted with dichloromethane
  2. washthe extract is washed with water
  3. customAfter drying the organic phase
  4. customover MgSO4 and evaporation
  5. customthe residue obtained
  6. customis purified

출처 및 근거

ORD 기록
ord-5ef060c277de4a7f95f86c5103556261
출처 데이터셋
uspto-grants-1999_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05945382

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