反应详情

温度

0 °C

To a solution of 9-Chloro-1-(2,4-dichlorophenyl)-6-[(ethylsulfanyl)methyl]-1,2,3,4-tetrahydropyrimido[1,2-a]benzimidazole (216 mg, 0.506 mmol) in acetonitrile (10 mL) was added 3-chloroperbenzoic acid (70%, 0.274 g, 1.11 mmol) at 0° C. The mixture was stirred at 0° C. for 1 hr. Aqueous sodium thiosulfate was added to the reaction mixture at 0° C. and the mixture was stirred at room temperature. The mixture was extracted with ethyl acetate. The organic layer was washed with aqueous sodium hydrogen carbonate and brine. The organic layer was concentrated in vacuo and the precipitated solid was collected by filtration. The solid was washed with water, 2-propanol and diisopropyl ether to give the title compound (190 mg, 0.414 mmol, 82%) as a colorless solid.

1. stirringthe mixture was stirred at room temperature
2. extractionThe mixture was extracted with ethyl acetate
3. washThe organic layer was washed with aqueous sodium hydrogen carbonate and brine
4. concentrationThe organic layer was concentrated in vacuo
5. filtrationthe precipitated solid was collected by filtration
6. washThe solid was washed with water, 2-propanol and diisopropyl ether