反应详情

10.6 g of ethyl 2-(4-methyl-2-pyridylthio)acetate (0.05 mole) and 8.8 g of 4-methoxy-1,2-phenylenediamine hydrochloride (0.05 mole) in 400 ml of 6N hydrochloric acid are heated under reflux for 2 days. The mixture is allowed to cool and is neutralized with ammonia solution. It is extracted with ethyl acetate (3×100 ml), and the extract is dried (Na2SO4), filtered and concentrated to a volume of 75 ml. From this solution, 8.4 g (59%) of 5-methoxy-2-(4-methyl-2-pyridylthiomethyl)benzimidazole, melting point 138°-140° C., crystallize. The data for the identification of the product appear in Tables 1 and 2.

1. temperatureunder reflux for 2 days
2. temperatureto cool
3. extractionIt is extracted with ethyl acetate (3×100 ml)
4. dry with materialthe extract is dried (Na2SO4)
5. filtrationfiltered
6. concentrationconcentrated to a volume of 75 ml
7. customFrom this solution, 8.4 g (59%) of 5-methoxy-2-(4-methyl-2-pyridylthiomethyl)benzimidazole, melting point 138°-140° C., crystallize