反应详情

2.0 Grams (7.0 mM) of 6-(3-bromopropoxy)-3,4-dihydrocarbostyril, 2.2 g (7.7 mM) of 2-methylimidazol and 1.3 ml (8.4 mM) of DBU were dissolved in 80 ml of isopropanol, and the resulting solution was refluxed by heating for 20 hours. The reaction mixture was concentrated, and to the resulting residue was added water, then extracted with chloroform. The chloroform extract was washed with water, dried with anhydrous sodium sulfate, then concentrated. The resulting residue was purified by means of a silica gel column chromatography (eluent: dichloromethane: methanol=20:1), and recrystallized from ethanol-n-hexane to yield 1.0 g of 6- [3-(2-methyl-1-imidazolyl)propoxy]-3,4-dihydrocarbostyril. White powdery substance. Melting point: 141.5°-142.5° C.

1. temperaturethe resulting solution was refluxed
2. temperatureby heating for 20 hours
3. concentrationThe reaction mixture was concentrated
4. additionto the resulting residue was added water
5. extractionextracted with chloroform
6. extractionThe chloroform extract
7. washwas washed with water
8. dry with materialdried with anhydrous sodium sulfate
9. concentrationconcentrated
10. customThe resulting residue was purified by means of a silica gel column chromatography (eluent: dichloromethane: methanol=20:1)
11. customrecrystallized from ethanol-n-hexane