反应详情

At room temperature, methyl 4-bromoacetylbenzoate (1.00 g) and thiourea (296 mg) were dissolved in isopropanol (100 ml), followed by heating under reflux for 15 minutes. Under stirring at the same temperature, anhydrous sodium carbonate (206 mg) was added to the reaction mixture. The resulting mixture was heated under reflux for 20 minutes. After completion of the reaction, water (50 ml) was added under ice cooling and the solid so precipitated was collected by filtration. The solid was dissolved in water and dichloromethane. The organic layer so separated was dried over anhydrous sodium sulfate. The solvent was then distilled off. The pale yellow solid so precipitated was washed with ether, whereby the title compound (634 mg, 70%) was obtained.

1. temperatureby heating
2. temperatureunder reflux for 15 minutes
3. additionwas added to the reaction mixture
4. temperatureThe resulting mixture was heated
5. temperatureunder reflux for 20 minutes
6. additionwas added under ice cooling
7. customthe solid so precipitated
8. filtrationwas collected by filtration
9. dissolutionThe solid was dissolved in water
10. customThe organic layer so separated
11. dry with materialwas dried over anhydrous sodium sulfate
12. distillationThe solvent was then distilled off
13. customThe pale yellow solid so precipitated
14. washwas washed with ether, whereby the title compound (634 mg, 70%)
15. customwas obtained