反应详情

5-(1-Piperazinyl)-3,4-dihydrocarbostyril (2.6 g) and 2 ml of trimethylamine were added to 40 ml of DMF. The mixture was stirred at room temperature while slowly adding dropwise 10 ml of DMF solution containing 2.4 g of 4-cyanobenzoyl chloride. After completion of addition, the reaction mixture was stirred at 40° to 50° C. for 30 minutes. The reaction mixture was poured into a large amount of water and extracted with chloroform. The extract was washed with sodium hydrogencarbonate solution and subsequently with water and dried over anhydrous sodium sulfate. Chloroform was distilled off and residual crystals were recrystallized from methanol-chloroform to give 1.9 g of 5-[4-(4-cyanobenzoyl)-1-piperazinyl]-3,4-dihydrocarbostyril, m.p. 266°-269° C., colorless granules.

1. additionAfter completion of addition
2. stirringthe reaction mixture was stirred at 40° to 50° C. for 30 minutes
3. extractionextracted with chloroform
4. washThe extract was washed with sodium hydrogencarbonate solution and subsequently with water
5. dry with materialdried over anhydrous sodium sulfate
6. distillationChloroform was distilled off
7. customresidual crystals were recrystallized from methanol-chloroform