反应详情

2-[[3-Methyl-4-(2,2,2-trifluoroethoxy)pyrid-2-yl]methylthio]benzimidazole (monohydrate) (10.0 g) was dissolved in ethanol (75 ml), to which was added a solution of sodium metavanadate (15 mg) in 35% aqueous solution of hydrogen peroxide (3.07 g), and allowed to react by stirring at 20°-25° for about 8 hours. After completion of the reaction an aqueous solution of sodium thiosulfate (1 g/5 ml) was added to the reaction mixture, which was stirred vigorously for about 10 minutes. The crystals were collected by filtration and washed with an ice-cooled mixture of ethanol-water (1:1). The crystals thus obtained were treated with a mixture of ethanol-water (9:1, 50 ml), heated (65°-70° C.) and stirred so that the crystals were dissolved, then the insoluble matters were removed by hot filtration. The filtrate was ice-cooled for crystallization, and the crystals were collected by filtration, washed with ice-cooled ethanol-water mixture (8:2) and dried in vacuo, to give white needles of 2-[[3-methyl-4-(2,2,2-trifluoroethoxy)pyrid-2-yl]methylsulfinyl]benzimidazole (9.0 g). (yield: 90.5%).

1. customto react
2. additionwas added to the reaction mixture, which
3. stirringwas stirred vigorously for about 10 minutes
4. filtrationThe crystals were collected by filtration
5. washwashed with an ice-
6. temperaturecooled
7. additionmixture of ethanol-water (1:1)
8. customThe crystals thus obtained
9. temperatureheated (65°-70° C.)
10. stirringstirred so that the crystals
11. dissolutionwere dissolved
12. customthe insoluble matters were removed by hot filtration
13. temperaturecooled for crystallization
14. filtrationthe crystals were collected by filtration
15. washwashed with ice-
16. temperaturecooled ethanol-water mixture (8:2)
17. customdried in vacuo