反应详情

1-(2,4-dihydroxyphenyl)ethanone (25.3 g, 0.17 mol) and 4-bromo-1-bromomethyl-2-fluorobenzene (44.6 g, 0.17 mol) were dissolved in DMF (150 mL). Potassium carbonate (11.8 g, 0.09 mol) was added to the solution under ice-cooled conditions, and the mixture was stirred under ice-cooled conditions and further stirred at room temperature for 12 hours. Again, potassium carbonate (11.8 g, 0.09 mol) was added to the mixture under ice-cooled conditions, and the mixture was stirred under ice-cooled conditions for 30 minutes and further stirred at room temperature for 12 hours. Methanol (100 mL) was added to this reaction solution, and the mixture was stirred at 80° C. for 1 hour. Thereafter, water (150 mL) was added to the mixture, and precipitated crystals were filtered and washed with methanol. The crystals were vacuum-dried at 60° C. for 2 hours, yielding 1-[4-(4-bromo-2-fluorobenzyloxy)-2-hydroxyphenyl]ethanone (43.5 g, yield: 75%).

1. temperaturecooled conditions
2. temperaturecooled conditions
3. stirringfurther stirred at room temperature for 12 hours
4. temperaturecooled conditions
5. stirringthe mixture was stirred under ice-
6. temperaturecooled conditions for 30 minutes
7. stirringfurther stirred at room temperature for 12 hours
8. stirringthe mixture was stirred at 80° C. for 1 hour
9. customprecipitated crystals
10. filtrationwere filtered
11. washwashed with methanol
12. customThe crystals were vacuum-dried at 60° C. for 2 hours