Reaktionsgleichung
[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]=1Komponenten
6
Reaktionsbedingungen
- Temperatur
- 120 °C
Versuchsvorschrift
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.
Aufarbeitung
- temperatureThe reaction solution was cooled
- filtrationthe insoluble matter was filtered off
- washthe filtrate was washed with water
- dry with materiala saturated saline solution and dried over an anhydrous magnesium sulfate
- distillationThe solvent was distilled off under reduced pressure
- customthe residue obtained
- customwas purified by silica gel column chromatography (eluent: hexane/ethyl acetate (98:2-80/20))
Quellen und Nachweise
- ORD-Eintrag
- ord-236a00b7ed9d4ccda644ca54e62e3c55
- Quelldatensatz
- uspto-grants-2013_02
- Patentnummer
- US08367708B2
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