反应详情

To a suspension of 6-[4-(3,4-dimethoxybenzoyl)-1-piperazinyl]-3,4-dihydrocarbostyril (10 g) in anhydrous tetrahydrofuran (250 ml) was added slowly n-butyllithium (20 ml, 1.5N hexane solution) with stirring and under ice-cooling. After completion of addition, the mixture was stirred at room temperature for 2 hours. Then, to the mixture was added slowly a solution of p-nitrobenzoyl chloride (6.1 g) in anhydrous tetrahydrofuran (25 ml) with stirring and under ice-cooling. After completion of addition, the mixture was stirred at the same temperature for 30 minutes. After completion of reaction, the reaction mixture was poured into water and extracted with chloroform. The chloroform layer was washed successively with water and saturated saline solution and dried over magnesium sulfate. The choloroform extract was evaporated under reduced pressure and the resultant residue was purified by silica-gel column chromatography (eluent:dichloromethane:methanol=100:1) to give 1-(4-nitrobenzoyl)-6-[4-(3,4-dimethoxybenzoyl)-1-piperazinyl]3,4-dihydrocarbostyril (2.6 g).

1. temperaturecooling
2. additionAfter completion of addition
3. stirringthe mixture was stirred at room temperature for 2 hours
4. stirringwith stirring and under ice-
5. temperaturecooling
6. additionAfter completion of addition
7. stirringthe mixture was stirred at the same temperature for 30 minutes
8. customAfter completion of reaction
9. extractionextracted with chloroform
10. washThe chloroform layer was washed successively with water and saturated saline solution
11. dry with materialdried over magnesium sulfate
12. extractionThe choloroform extract
13. customwas evaporated under reduced pressure
14. customthe resultant residue was purified by silica-gel column chromatography (eluent:dichloromethane:methanol=100:1)