反应详情

A solution of 11-cyano-11-[3-(dimethylamino)propyl]-6,11-dihydrodibenz[b,e]oxepin of Example 4 (3.0 g; 0.009 mole) in dry ether is vigorously stirred and cooled in an ice bath. A saturated solution of HCl in ether is added dropwise until no more salt precipitates. The salt is filtered, washed with ether and dried. Two recrystallizations from methanol-ether provide 1.1 g of crystals of 11-cyano-11-[3-dimethylamino)propyl[-6,11-dihydrodibenz[b,e]oxepin hydrochloride, m.p. 219° C.

1. temperaturecooled in an ice bath
2. customprecipitates
3. filtrationThe salt is filtered
4. washwashed with ether
5. customdried
6. customTwo recrystallizations from methanol-ether