反应详情

To a suspension of 0.2 g (0.74 mmol) of 10,11-dihydro-10-hydroxyimino-5H-dibenz[b,f]azepine-5-carboxamide and 0.01 g (0.08 mmol) of 4-dimethylaminopyridine in 10 mL of dichloromethane and 0.29 g (3.7 mmol) of pyridine was added 0.28 g (2.6 mmol) of ethyl chloroformate dropwise. The resulting mixture was stirred at room temperature for 2 hours whereupon it was extracted with 20 mL of 1M aqueous HCl and a saturated solution of NaHCO3, then dried by sodium sulphate and filtered. The solvent was removed by evaporation under reduced pressure and the residue was crystallised from a mixture of dichloromethane and ethyl acetate to give white crystals of m.p. 188.9°-190° C.

1. extractionwas extracted with 20 mL of 1M aqueous HCl
2. dry with materiala saturated solution of NaHCO3, then dried by sodium sulphate
3. filtrationfiltered
4. customThe solvent was removed by evaporation under reduced pressure
5. customthe residue was crystallised from a mixture of dichloromethane and ethyl acetate
6. customto give white crystals of m.p. 188.9°-190° C.