Hydrogen Peroxide → HCID 19598444, compound

Participants

Reaction Conditions

Reaction Steps

Forty mg. of acetylacetone vanadium(IV) was dissolved in 150 ml. of ethanol, followed by addition of 20.0 g. of 2-[[3-methyl-4-(2,2,2-trifluoroethoxy)-pyridin-2-yl]methylthio]benzimidazole monohydride and further dropwise addition of 6.14 g. of 35% aqueous hydrogen peroxide solution at 20 to 25° C. The mixture was allowed to react at the same tempertaure for about 5 hours. After completion of the reaction, aqueous solution of sodium thiosulfate(2.7 g./16 ml.) was added, followed by vigorous stirring for about 10 minutes. The precipitated crystals were collected by filtration and washed with ice-cooled ethanol-water mixture (8:2). To the resultant crystals was added 90 ml. of ethanol-water mixture(9:1), and the mixture was heated to 60 to 70° C. under stirring to dissolve the crystals. The insolubles were filtered off while the mixture was hot. The filtrate was ice-cooled to precipitate crystals. The precipitated crystals were collected by filtration, washed with ice-cooled ethanol-water(8:2) and dried under reduced pressure at room temperature to give 2-[[3-methyl-4-(2,2,2-trifluoroethoxy)pyridin-2-yl]methylsulfinyl]-benzimidazole monohydrate, monoethanolate solvate as white needles. Yield:21.2 g.(91.0%).

Provenance & Evidence