反应详情

5-(2-Chlorophenyl)-7-ethyl-2-hydrazino-3H-thieno[2,3-e] [1,4]diazepine (20 g) was suspended in chloroform (200 ml) at room temperature. Cyclohexanecarboxylic acid chloride (10.1 g) was added, and the mixture was stirred for 3 hours. The reaction mixture was washed with a saturated aqueous sodium hydrogencarbonate solution and saturated brine, and dried over magnesium sulfate. The solvent was evaporated to give an oil. The oil was dissolved in a mixed solvent of toluene (200 ml) and acetic acid (5.4 ml), and the mixture was refluxed for 3 hours. The reaction mixture was washed with a saturated aqueous sodium hydrogencarbonate solution and saturated brine and dried over magnesium sulfate. The solvent was evaporated. The residue was purified by silica gel column chromatography (eluted with ethyl acetate), and isopropyl ether was added to give 15 g of 4-(2-chlorophenyl)-9-cyclohexyl-2-ethyl-6H-thieno[3,2-f] [1,2,4]triazolo[4,3-a] [1,4]diazepine.

1. washThe reaction mixture was washed with a saturated aqueous sodium hydrogencarbonate solution and saturated brine
2. dry with materialdried over magnesium sulfate
3. customThe solvent was evaporated
4. customto give an oil
5. temperaturethe mixture was refluxed for 3 hours
6. washThe reaction mixture was washed with a saturated aqueous sodium hydrogencarbonate solution and saturated brine
7. dry with materialdried over magnesium sulfate
8. customThe solvent was evaporated
9. customThe residue was purified by silica gel column chromatography (eluted with ethyl acetate), and isopropyl ether
10. additionwas added