反应详情

A solution of 330 mg of 6-[[(4-methoxy-3-methyl-2-pyridyl)methyl]thio]-5H-1,3-dioxolo[4,5-f]benzimidazole in 5 ml of chloroform was treated portionwise with 200 mg of m-chloroperbenzoic acid while cooling with ice and stirring. After 15 minutes the reaction mixture was extracted with 10% sodium carbonate solution, dried and concentrated. The residue was chromatographed on silica gel with methylene chloride/methanol (8.5:1.5) as the elution agent, the medium pressure flash chromatography method being used and the pressure being produced with nitrogen. By recrystallization from ether there was obtained 6-[[(4-methoxy-3-methyl-2-pyridyl)methyl]sulfinyl]-5H-1,3-dioxolo[4,5-f]benzimidazole of melting point 185°-186° (decomposition).

1. temperaturewhile cooling with ice
2. extractionAfter 15 minutes the reaction mixture was extracted with 10% sodium carbonate solution
3. customdried
4. concentrationconcentrated
5. customThe residue was chromatographed on silica gel with methylene chloride/methanol (8.5:1.5) as the elution agent
6. customthe pressure being produced with nitrogen
7. customBy recrystallization from ether