反应详情

4-(2-Chlorophenyl)-2-ethyl-6H-thieno[3,2-f] [1,2,4]triazolo[4,3-a] [1,4]diazepine (10 g) was dissolved in dichloroethane (100 ml), and bromine (1.7 ml) was added under ice-cooling. The mixture was heated to room temperature, and allowed to stand overnight. The solvent was evaporated, and chloroform was added. The mixture was washed with an aqueous sodium thiosulfate solution, a saturated aqueous sodium hydrogencarbonate solution and brine, and dried over magnesium sulfate. The solvent was evaporated, and the residue was purified by silica gel column chromatography (developing solvent:ethyl acetate-hexane) and crystallized from ethyl acetate to give 3.4 g of 9-bromo-4-(2-chlorophenyl)-2-ethyl-6H-thieno[3,2-f] [1,2,4]triazolo[4,3-a] [1,4]diazepine.

1. temperaturecooling
2. customThe solvent was evaporated
3. additionchloroform was added
4. washThe mixture was washed with an aqueous sodium thiosulfate solution
5. dry with materiala saturated aqueous sodium hydrogencarbonate solution and brine, and dried over magnesium sulfate
6. customThe solvent was evaporated
7. customthe residue was purified by silica gel column chromatography (developing solvent:ethyl acetate-hexane)
8. customcrystallized from ethyl acetate