反应详情

3,4-Dimethoxybenzoic acid (2.6 g) and 1.65 g of 1,8-diazabicyclo[5,4,0]undecene-7 were added to 100 ml of DMF and to the mixture was added dropwise 1.5 ml of isobutyl chloroformate with ice-cooling externally with stirring. After completion of addition, the mixture was stirred for 30 minutes. To the mixture was added 40 ml of DMF solution containing 2.16 g of 5-(1-piperazinyl)oxindol and the mixture was stirred at room temperature for 5 hours. After completion of reaction, the solvent was removed by distillation. The residue was extracted with 300 ml of chloroform and the extract was washed with a diluted aqueous solution of sodium hydrogencarbonate, water, diluted hydrochloric acid and water, successively. Chloroform was removed by distillation and the residue was recrystallized from methanol to give 1.6 g of 5-[4-(3,4-dimethoxybenzoyl)-1-piperazinyl]oxindol.

1. temperaturecooling externally
2. additionAfter completion of addition
3. stirringthe mixture was stirred for 30 minutes
4. stirringthe mixture was stirred at room temperature for 5 hours
5. customAfter completion of reaction
6. customthe solvent was removed by distillation
7. extractionThe residue was extracted with 300 ml of chloroform
8. washthe extract was washed with a diluted aqueous solution of sodium hydrogencarbonate, water, diluted hydrochloric acid and water
9. customChloroform was removed by distillation
10. customthe residue was recrystallized from methanol