反应详情

2.5 g (6 mmol) of 2-chloromethyl-3-methyl-4-{4-[2-(2-methyl-5-nitroimidazol-1-yl)ethylthio]butylthio}-pyridine and 0.9 g (6 mmol) of 2-mercaptobenzimidazole are heated to reflux for 1 h in 25 ml of isopropanol. The mixture is then cooled in an ice bath and the precipitated solid is filtered off with suction. The solid is taken up in water and treated with saturated sodium hydrogen carbonate solution. The mixture is extracted with dichloromethane. The organic phase is washed with water, dried over magnesium sulfate, filtered and concentrated. The title compound crystallizes and is washed with a little methanol with stirring. M.p. 160°-162° C.; yield 0.62 g (20% of theory).

1. temperatureThe mixture is then cooled in an ice bath
2. filtrationthe precipitated solid is filtered off with suction
3. additiontreated with saturated sodium hydrogen carbonate solution
4. extractionThe mixture is extracted with dichloromethane
5. washThe organic phase is washed with water
6. dry with materialdried over magnesium sulfate
7. filtrationfiltered
8. concentrationconcentrated
9. customThe title compound crystallizes
10. washis washed with a little methanol