反应详情

5-(1-Piperazinyl)oxindol.hydrobromide (2.0 g) was suspended in 30 ml of N,N-dimethylformamide (DMF), and 2.3 ml of triethylamine was added thereto subsequently. The mixture was cooled to 0° to 5° C. To the mixture was added dropwise 5 ml of DMF solution containing 1.5 g of 3,4-dimethoxybenzoyl chloride at the same temperature as above with stirring. After completion of addition, the mixture was stirred at room temperature for one hour. The reaction mixture was poured into a large amount of water and extracted with chloroform. After washing with water, the extract was dried over anhydrous sodium sulfate and chloroform was removed by distillation. The residue was purified by silica-gel column chromatography (eluent: chloroform:methanol=100:1) and recrystallized from methanol to give 1.5 g of 5-[4-(3,4-dimethoxybenzoyl)-1-piperazinyl]oxindol.

1. temperatureThe mixture was cooled to 0° to 5° C
2. additionAfter completion of addition
3. stirringthe mixture was stirred at room temperature for one hour
4. extractionextracted with chloroform
5. washAfter washing with water
6. dry with materialthe extract was dried over anhydrous sodium sulfate and chloroform
7. customwas removed by distillation
8. customThe residue was purified by silica-gel column chromatography (eluent: chloroform:methanol=100:1)
9. customrecrystallized from methanol