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Chlorodifluoromethane → HCID 21852637、化合物

HRID 1586351
ノート
印刷プレビュー

反応式

HRID 1586351 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

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

生成物 1

HCID 21852637HCID 21852637、化合物収率 21%

試薬・触媒・溶媒 2

HCID 94433Tetrabutylammonium hydrogen sulfate触媒HCID 6344Dichloromethane
溶媒

実験手順

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%.

後処理

  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

出典と根拠

ORDレコード
ord-5ef060c277de4a7f95f86c5103556261
出典データセット
uspto-grants-1999_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05945382

反応ノート

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