反应详情

温度

80 °C

A mixture of 2.20 g of 2-chloro-11-(1-piperazinyl)dibenz[b,f][1,4]oxazepine, 0.76 g of ethyl chloroformate and 0.97 g of potassium carbonate in 20 ml of N,N-dimethylformamide was stirred at 80° C. for 3 hrs. Ice water was added to the reaction mixture and extracted with ether. The etheral layer was washed with water, dried and concentrated. The residue was chromatographed on silica gel using a mixture of n-hexane and ethyl acetate (1:2) as eluents to give 2.62 g of colorless crystals, which were recrystallized from isopropyl ether to give colorless prisms, mp 121.5°-122.5° C.

1. extractionextracted with ether
2. washThe etheral layer was washed with water
3. customdried
4. concentrationconcentrated
5. customThe residue was chromatographed on silica gel using
6. additiona mixture of n-hexane and ethyl acetate (1:2) as eluents