HRID261553
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
g 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 pale brown prismatic crystals having a melting point of 175°-177° C.
WORKUP
后处理
- temperaturethe resulting mixture was heated
- temperatureunder reflux for 3.5 hours
- concentrationThe reaction mixture was concentrated to 5 ml
- customto separate crystals
- temperatureon cooling
- filtrationwhich were collected by filtration
- customRecrystallization from ethanol