反应详情

A solution of 330 mg (1 mmol) of 6-[[(4-methoxy-3-methyl-2-pyridyl)methyl]thio]-5H-1,3-dioxolo[4,5-f]-benzimidazole in 5 ml of chloroform is treated portionwise with 200 mg (1.2 mmol) of m-chloroperbenzoic acid While cooling with ice and stirring. After 15 minutes the reaction mixture is extracted with 10% sodium carbonate solution, dried and concentrated. The residue is 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 is obtained 6-[[(4-methoxy-3-methyl -2-pyridyl)methyl]sulphinyl]-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 is extracted with 10% sodium carbonate solution
3. customdried
4. concentrationconcentrated
5. customThe residue is 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