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

HRID 384148

反応式

HRID 384148 の反応式
[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

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 679Dimethyl Sulfoxide溶媒

反応条件

温度
120 °C

実験手順

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.

後処理

  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))

出典と根拠

ORDレコード
ord-236a00b7ed9d4ccda644ca54e62e3c55
出典データセット
uspto-grants-2013_02
特許番号
US08367708B2

関連ノート

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