反应详情

温度

70 °C

To a stirred solution of 3-(3-chloro-1-methylpropyl)-7-(1,3-dimethyl-1H-pyrazol-5-yl)-2,3,4,5-tetrahydro-1H-3-benzazepine (0.10 g) (intermediate 10) and 4-methyl-5-(2-methyl-5-quinolinyl)-2,4-dihydro-3H-1,2,4-triazole-3-thione (0.093 g) (intermediate 7) in dimethylformamide (2 ml), at room temperature, sodium iodide (0.040 g) and anhydrous potassium carbonate were subsequently added. Then the reaction mixture was warmed to 70° C. and stirring continued for 3 h after which time the mixture was allowed to reach room temperature and the solvent evaporated under reduced pressure. The residue was treated with water (10 ml), extracted with ethyl acetate (20 ml). The organic phase was dried with sodium sulphate and after evaporation the crude product was purified by chromatography on silica gel with 100-95% dichloromethane-methanol elution to give 7-(1,3-dimethyl-1H-pyrazol-5-yl)-3-(1-methyl-3-{[4-methyl-5-(2-methyl-5-quinolinyl)-4H-1,2,4-triazol-3-yl]thio}propyl)-2,3,4,5-tetrahydro-1H-3-benzazepine (0.040 g) as a pale yellow solid. This product was dissolved in dichloromethane (2 ml), and hydrochloridric acid was added dropwise (0.072 ml, 1M/ether), at room temperature. Following solvent evaporation gave the title compound (0.042 g) as a yellow solid.

1. customto reach room temperature
2. customthe solvent evaporated under reduced pressure
3. additionThe residue was treated with water (10 ml)
4. extractionextracted with ethyl acetate (20 ml)
5. dry with materialThe organic phase was dried with sodium sulphate
6. customafter evaporation the crude product
7. customwas purified by chromatography on silica gel with 100-95% dichloromethane-methanol elution