Ethyl Acetate → 2-Chloro-1-(4-iodophenoxy)-4-(trifluoromethyl)benzene

HRID 384148

반응식

HRID 384148 반응식
[I:1][C:2]1[CH:7]=[CH:6][C:5]([OH:8])=[CH:4][CH:3]=1.[Cl:9][C:10]1[CH:15]=[C:14]([C:16]([F:19])([F:18])[F:17])[CH:13]=[CH:12][C:11]=1F.C(=O)([O-])[O-].[K+].[K+].C(OCC)(=O)C>CS(C)=O>[Cl:9][C:10]1[CH:15]=[C:14]([C:16]([F:17])([F:18])[F:19])[CH:13]=[CH:12][C:11]=1[O:8][C:5]1[CH:6]=[CH:7][C:2]([I:1])=[CH:3][CH:4]=1

참가 물질

6

반응물 4

HCID 8857Ethyl AcetateHCID 108944-IodophenolHCID 11430Potassium CarbonateHCID 157153Benzene, 2-chloro-1-fluoro-4-(trifluoromethyl)-

생성물 1

HCID 684307232-Chloro-1-(4-iodophenoxy)-4-(trifluoromethyl)benzene

시약·촉매·용매 1

HCID 679Dimethyl Sulfoxide용매

반응 조건

온도
120 °C

실험 절차

To a solution of 4-iodophenol (200 mg) in dimethylsulfoxide (1 ml), 218 mg of 2-chloro-1-fluoro-4-(trifluoromethyl)benzene and 251 mg of potassium carbonate were added, and the reaction solution was stirred at 120° C. for 3 hours. The reaction solution was cooled, ethyl acetate was added, the insoluble matter was filtered off, and the filtrate was washed with water and a saturated saline solution and dried over an anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure, and the residue obtained was purified by silica gel column chromatography (eluent: hexane/ethyl acetate (98:2-80/20)) to afford the title compound as a colorless oil.

후처리

  1. temperatureThe reaction solution was cooled
  2. filtrationthe insoluble matter was filtered off
  3. washthe filtrate was washed with water
  4. dry with materiala saturated saline solution and dried over an anhydrous magnesium sulfate
  5. distillationThe solvent was distilled off under reduced pressure
  6. customthe residue obtained
  7. customwas purified by silica gel column chromatography (eluent: hexane/ethyl acetate (98:2-80/20))

출처 및 근거

ORD 기록
ord-236a00b7ed9d4ccda644ca54e62e3c55
출처 데이터셋
uspto-grants-2013_02
특허 번호
US08367708B2

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