反应详情

To 4.6 g of 6,7-dihydro-1H-p-dioxino(2,3-f)benzimidazole-2-thiol, suspended in 50 ml of alcohol, were added dropwise while stirring 1.8 g of sodium hydroxide in 25 ml of water and, after 30 minutes, there were added 3.7 g of 2-chloromethyl-pyridine hydrochloride. The mixture was left to boil at reflux overnight, it was then evaporated, and the residue was taken up in methylene chloride. This mixture was washed first with 3 N sodium hydroxide, then neutral with water, dried over sodium sulfate and evaporated in vacuo. The crude product was recrystallized from ethyl acetate/petroleum ether. 3.5 g (53% of theory) of 6,7-dihydro-2-[(2-pyridylmethyl)thio]-1H-p-dioxino(2,3-f)benzimidazole of melting point 155°-156° C. were prepared.

1. additionwere added dropwise
2. waitThe mixture was left
3. temperatureat reflux overnight
4. customit was then evaporated
5. washThis mixture was washed first with 3 N sodium hydroxide
6. dry with materialneutral with water, dried over sodium sulfate
7. customevaporated in vacuo
8. customThe crude product was recrystallized from ethyl acetate/petroleum ether