反应详情

温度

140 °C

4-(4-Fluorobenzoyl)-1,3-dihydro-5-methyl-2H-imidazol-2-one (6.6 g 30 mmol) is combined with 4-methyl-1H-imidazole (33 g, ca. 400 mmol) in a sealed flask and the mixture heated with stirring at ca. 140° C. overnight. The mixture is cooled, water (120 mL) added and the mixture stirred in an ice bath. The suspension is filtered and the filter cake washed with water and acetone. The solid is heated under reflux in a mixture of 2-propanol (300 mL) and water (200 mL) until dissolution is complete. The solution is filtered, reheated to dissolve some precipitated solid and allowed to cool slowly to room temperature. After 2.5 days the mixture is cooled in ice for 2 hr, the solid collected by filtration, washed with acetone, and dried in vacuo at 105° C. for 23 hr to produce the title compound.

1. temperaturethe mixture heated
2. temperatureThe mixture is cooled
3. stirringthe mixture stirred in an ice bath
4. filtrationThe suspension is filtered
5. washthe filter cake washed with water and acetone
6. temperatureThe solid is heated
7. temperatureunder reflux in a mixture of 2-propanol (300 mL) and water (200 mL) until dissolution
8. filtrationThe solution is filtered
9. dissolutionto dissolve some precipitated solid
10. temperatureto cool slowly to room temperature
11. temperatureAfter 2.5 days the mixture is cooled in ice for 2 hr
12. filtrationthe solid collected by filtration
13. washwashed with acetone
14. customdried in vacuo at 105° C. for 23 hr