反应详情

2.4 Grams (13.4 mM) of 6-mercapto-3,4-dihydrocarbostyril, 3,3 g (17.4 mM) of 1-(3-bromopropyl)-1,2,4-triazol, and 2.6 ml (17.4 mM) of DBU were added to 60 ml of isopropanol, and the whole mixture was refluxed by heating for 2 hours. After the reaction was completed, the reaction mixture was concentrated, the resulting residue was extracted with chloroform. The chloroform extract was washed with water, an aqueous solution saturated with sodium hydrogen carbonate, and water in this order, then dried with anhydrous sodium sulfate. The dried extract was concentrated by removing the solvent by evaporation, the residue was purified by means of a silica gel column chromatography (eluent: dichloromethane:methanol=20:1), and recrystallized from ethanol-n-hexane to yield 2.5 g of 6-[3-(1H-1,2,4-triazol-1-yl)propylthio]-3,4-dihydrocarbostyril. Colorless needle-like crystals. Melting point: 114.5°-115.5° C.

1. temperaturethe whole mixture was refluxed
2. temperatureby heating for 2 hours
3. concentrationthe reaction mixture was concentrated
4. extractionthe resulting residue was extracted with chloroform
5. extractionThe chloroform extract
6. washwas washed with water
7. dry with materialan aqueous solution saturated with sodium hydrogen carbonate, and water in this order, then dried with anhydrous sodium sulfate
8. extractionThe dried extract
9. concentrationwas concentrated
10. customby removing the solvent
11. customby evaporation
12. customthe residue was purified by means of a silica gel column chromatography (eluent: dichloromethane:methanol=20:1)
13. customrecrystallized from ethanol-n-hexane