반응 #157743

반응 방정식

water

2,2,2-Trifluoroethyliodide

potassium carbonate

4-bromo-2-chlorophenol

→

4-bromo-2-chloro-1-(2,2,2-trifluoroethoxy)benzene

수율 43.0%

용매

N,N-dimethylformamide

반응 조건

후처리

1. 1
   온도The reaction solution was cooled to room temperature
2. 2
   추출followed by extraction with ethyl acetate
3. 3
   세척The organic layer was washed with brine
4. 4
   건조dried over anhydrous magnesium sulfate
5. 5
   여과filtered
6. 6
   기타The solvent was then evaporated under reduced pressure
7. 7
   기타The residue was purified by silica gel column chromatography (hexane only)

실험 절차

2,2,2-Trifluoroethyliodide (15.2 g) and potassium carbonate (10.0 g) were added to a solution of 4-bromo-2-chlorophenol (5.0 g) in N,N-dimethylformamide (20 mL), and the mixture was stirred at 80° C. for 20 hours. The reaction solution was cooled to room temperature and water was added, followed by extraction with ethyl acetate. The organic layer was washed with brine, dried over anhydrous magnesium sulfate and filtered. The solvent was then evaporated under reduced pressure. The residue was purified by silica gel column chromatography (hexane only) to give 4-bromo-2-chloro-1-(2,2,2-trifluoroethoxy)benzene as a colorless oil (3.0 g, 43%).

출처