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Water → 2-Phenoxy-4-trifluoroacetylfluorobenzene

HRID 975217
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HRID 975217 반응식
[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
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 962WaterHCID 19971591HCID 19971591, 화합물HCID 23665760Sodium Hypochlorite

생성물 1

HCID 199715862-Phenoxy-4-trifluoroacetylfluorobenzene

시약·촉매·용매 2

HCID 94433Tetrabutylammonium hydrogen sulfate촉매HCID 6344Dichloromethane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-b40a74212fbe442891043a75d060a2d9
출처 데이터셋
uspto-grants-1997_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05608062

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