反应详情

1.0 g of 2-mercapto-5-(2,2,2-trifluoroethoxy)-1H-benzimidazole is dissolved in 15 ml of ethanol and 8.5 ml of 1N sodium hydroxide solution, 0.90 g of 2-chloromethyl-4,5-dimethoxypyridinium chloride are added and the mixture is stirred for 20 hours. After addition of 30 ml of water, the mixture is extracted three times with 30 ml of methylene chloride each time, the methylene chloride phase is washed once with 5 ml of 0.1N sodium hydroxide solution, the combined organic phases are dried over magnesium sulfate and, after the drying agent has been filtered off, the filtrate is completely concentrated. 1.51 g (94% of theory) of the title compound are obtained as an amorphous solid residue of m.p. 55°-57° C.

1. extractionthe mixture is extracted three times with 30 ml of methylene chloride each time
2. washthe methylene chloride phase is washed once with 5 ml of 0.1N sodium hydroxide solution
3. dry with materialthe combined organic phases are dried over magnesium sulfate
4. filtrationafter the drying agent has been filtered off
5. concentrationthe filtrate is completely concentrated