反应详情

In 10 ml of tetrahydrofuran were dissolved 0.52 g (0.002 mole) of the 2-(1-imidazolyl)-2-(4-chloromethyl-1,3-dithiolan-2-ylidene)acetonitrile obtained in Example 2 and 0.31 g of 1,8-diazabicyclo-[5,4,0]-7-undecene, and the reaction was carried out with heating under reflux for 1 hour. After the reaction solution was allowed to cool, the deposited salt was separated by filtration and the filtrate was concentrated to obtain crude crystals, which were then recrystallized from ethyl acetate-n-hexane to obtain 0.35 g of the desired compound in the form of crystals: melting point 115.7° C., yield 79%.

1. temperaturewith heating
2. temperatureunder reflux for 1 hour
3. temperatureto cool
4. customthe deposited salt was separated by filtration
5. concentrationthe filtrate was concentrated
6. customto obtain crude crystals, which
7. customwere then recrystallized from ethyl acetate-n-hexane