反应详情

0.9 g of 9-cyano-10,11-dihydro-11-oxo-dibenzo[b,f]thiepin and 1 g of 100% hydrazine hydrate were dissolved in 10 ml of ethanol and the resulting mixture was heated under reflux for 3.5 hours. The reaction mixture was concentrated to 5 ml to separate crystals on cooling, which were collected by filtration. Recrystallization from ethanol afforded 0.6 g of 9-cyano-10,11-dihydro-11-oxo-dibenzo[b,f]thiepin hydrazone as palo brown prismatic crystals having a melting point of 175°-177° C.

1. temperaturethe resulting mixture was heated
2. temperatureunder reflux for 3.5 hours
3. concentrationThe reaction mixture was concentrated to 5 ml
4. customto separate crystals
5. temperatureon cooling
6. filtrationwhich were collected by filtration
7. customRecrystallization from ethanol