反应详情

Ethyl chloroformate (19.53 g) was added dropwisely to a solution of 9.52 g of 1,2,3,4,10,14b-hexahydro-2-methyldibenzo[c,f]pyrazino[1,2-a]azepine in 48 ml of benzene at refluxed temperature and the mixture was refluxed for 5 hrs. Ice water was added to the reaction mixture and made alkaline with sodium bicarbonate. The mixture was extracted with benzene and the benzene layer was washed with water, dried and concentrated. The residue was chromatographed on silica gel using a mixture of n-hexane and ethyl acetate as an eluent (1:2) to give 8.70 g of pale yellow crystals, which were recrystallized from a mixture of isopropyl ether and n-pentane to give pale yellow prisms, mp 108.5°-109.5° C.

1. temperatureat refluxed temperature
2. temperaturethe mixture was refluxed for 5 hrs
3. extractionThe mixture was extracted with benzene
4. washthe benzene layer was washed with water
5. customdried
6. concentrationconcentrated
7. customThe residue was chromatographed on silica gel using
8. additiona mixture of n-hexane and ethyl acetate as an eluent (1:2)