反应详情

8-(1-Piperazinyl)carbostyril (0.7 g, 2.26 mmols) and sodium hydrogencarbonate (0.2 g) were suspended in 5 ml of DMF and the suspension was stirred at room temperature for 30 minutes. To the resulting mixture was added 0.4 ml of triethylamine, and further a solution of 0.47 g of 2-chlorobenzoyl chloride in 5 ml of DMF dropwise, followed by stirring at room temperature for 30 minutes. The reaction mixture was poured in saturated aqueous sodium hydrogencarbonate and extracted with chloroform. The organic layer was washed with water and then with saturated aqueous sodium hydrogencarbonate and dried over sodium sulfate. After distilling off the solvent, ether was added to the residue to crystallize. The crystals thus obtained were recrystallized from ethanol to give 0.24 g of 8-[4-(2-chlorobenzoyl)-1-piperazinyl]carbostyril, m.p. 239°-240.5° C., colorless needles.

1. stirringby stirring at room temperature for 30 minutes
2. extractionextracted with chloroform
3. washThe organic layer was washed with water
4. dry with materialwith saturated aqueous sodium hydrogencarbonate and dried over sodium sulfate
5. distillationAfter distilling off the solvent, ether
6. additionwas added to the residue
7. customto crystallize
8. customThe crystals thus obtained
9. customwere recrystallized from ethanol