反应详情

350 ml of thionyl chloride are added dropwise at a temperature of 30 to 40° to a solution of 201.5 g of crude 10,11-dihydro-5H-dibenzo[a,d]cyclohepten-5-ol in 700 ml of dry benzene over a period of 40 minutes. Subsequently, the mixture is heated to boiling under reflux for an additional 1.5 hours and concentrated in vacuo. The residue is diluted 2 to 3 times with 300 ml of benzene each time and in each case again evaporated. There is obtained 5-chloro-10,11-dihydro-5H-dibenzo[a,d]cycloheptene as a beige crystalline mass of melting point 99-101° which is used in the next step without further purification. By recrystallization from carbon tetrachloride there is obtained material of melting point 104°-105° C.

1. temperatureSubsequently, the mixture is heated
2. temperatureunder reflux for an additional 1.5 hours
3. concentrationconcentrated in vacuo
4. additionThe residue is diluted 2 to 3 times with 300 ml of benzene each time
5. customin each case again evaporated