反应详情

To solution of 3-chloro-4-(trifluoromethyl)benzyl bromide (300 mg, 1.097 mmol) in acetone (15 mL) was added 4-bromo-2,5-difluorophenol (1.097 mmol) followed by potassium carbonate (303 mg, 2.194 mmol). The reaction mixture was heated at reflux for 3.5 hours and then allowed to cool to room temperature. The solvent was removed under reduced pressure to yield a white solid, which was partitioned with water/EtOAc mixture (1:1, 50 mL). The organic layer was separated and the aqueous was extracted with EtOAc (3×30 mL). The combined organics were washed with brine (50 mL), dried over sodium sulphate, filtered and concentrated in vacuo to give the title compound as a white solid (434 mg, 99%).

1. temperatureThe reaction mixture was heated
2. temperatureat reflux for 3.5 hours
3. customThe solvent was removed under reduced pressure
4. customto yield a white solid, which
5. customwas partitioned with water/EtOAc mixture (1:1, 50 mL)
6. customThe organic layer was separated
7. extractionthe aqueous was extracted with EtOAc (3×30 mL)
8. washThe combined organics were washed with brine (50 mL)
9. dry with materialdried over sodium sulphate
10. filtrationfiltered
11. concentrationconcentrated in vacuo