反应详情

温度

20 °C

0.96 g of 2-chloromethyl-4,5-dimethoxy-3-methylpyridinium chloride are added to a solution of 0.92 g of 2,2-difluoro-5H-[1,3]-dioxolo[4,5-f]benzimidazole-6-thiol in 10 ml of ethanol and 10 ml of 1N sodium hydroxide solution. The yellow reaction mixture is stirred at 20° C. for 1 hour, a further 10 ml of water are added, whereupon a colorless solid precipitates out, the mixture is stirred for a further 5 hours and filtered and the residue is rinsed with 1N sodium hydroxide solution and water and dried to constant weight. The amorphous powder is recrystallized from methylene chloride/diisopropyl ether. 1.5 g (93% of theory) of the title compound are obtained in the form of colorless crystals of m.p. 160°-161° C.

1. customprecipitates out, the mixture
2. stirringis stirred for a further 5 hours
3. filtrationfiltered
4. washthe residue is rinsed with 1N sodium hydroxide solution and water
5. customdried to constant weight
6. customThe amorphous powder is recrystallized from methylene chloride/diisopropyl ether