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Water → 2-Phenoxy-4-trifluoroacetylfluorobenzene

HRID 975217
ノート
印刷プレビュー

反応式

HRID 975217 の反応式
[F:1][C:2]([F:20])([F:19])[CH:3]([C:5]1[CH:10]=[CH:9][C:8]([F:11])=[C:7]([O:12][C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)[CH:6]=1)[OH:4].Cl[O-].[Na+].O>S([O-])(O)(=O)=O.C([N+](CCCC)(CCCC)CCCC)CCC.C(Cl)Cl>[O:12]([C:7]1[CH:6]=[C:5]([C:3](=[O:4])[C:2]([F:1])([F:19])[F:20])[CH:10]=[CH:9][C:8]=1[F:11])[C:13]1[CH:14]=[CH:15][CH:16]=[CH:17][CH:18]=1
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 962WaterHCID 19971591HCID 19971591、化合物HCID 23665760Sodium Hypochlorite

生成物 1

HCID 199715862-Phenoxy-4-trifluoroacetylfluorobenzene

試薬・触媒・溶媒 2

HCID 94433Tetrabutylammonium hydrogen sulfate触媒HCID 6344Dichloromethane溶媒

実験手順

14.37 g (0.05 mol) of 2,2,2-trifluoro-1-(4-fluoro-3-phenoxyphenyl)ethanol and 0.85 g (0.0025 mol) of tetrabutylammonium hydrogen sulfate are dissolved in 200 ml of methylene chloride at room temperature. 31 ml (0.06 mol) of an approximately 12% strength sodium hypochlorite solution are metered in within 20 minutes with vigorous stirring and the mixture is stirred for a further 6 hours at room temperature. The reaction mixture is added to 200 ml of water, the phases are separated, the aqueous phase is extracted several times with methylene chloride and the combined organic phases are washed with saturated aqueous sodium chloride solution. After drying the organic phase with sodium sulfate, the volatiles are distilled off. Following distillation of the crude product in a kugelrohr (0.2 mbar, 150°-165° C. bath temperature), 10.8 g (76% of theory) of 2-phenoxy-4-trifluoroacetylfluorobenzene are obtained. nD20 : 1.5230.

後処理

  1. customare metered in within 20 minutes
  2. stirringthe mixture is stirred for a further 6 hours at room temperature
  3. customthe phases are separated
  4. extractionthe aqueous phase is extracted several times with methylene chloride
  5. washthe combined organic phases are washed with saturated aqueous sodium chloride solution
  6. dry with materialAfter drying the organic phase with sodium sulfate
  7. distillationthe volatiles are distilled off
  8. distillationdistillation of the crude product in a kugelrohr (0.2 mbar, 150°-165° C. bath temperature), 10.8 g (76% of theory) of 2-phenoxy-4-trifluoroacetylfluorobenzene
  9. customare obtained

出典と根拠

ORDレコード
ord-b40a74212fbe442891043a75d060a2d9
出典データセット
uspto-grants-1997_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05608062

反応ノート

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