反应详情

2-Nitro-5-piperazinylbenzaldehyde (5 g) was suspended in 50 ml of DMF and 6 ml of triethylamine was added to the suspension. A solution of 4.4 g of 3,4-dimethoxybenzoyl chloride in 20 ml of DMF was added dropwise thereto with ice cooling externally while stirring and the mixture was stirred at room temperature for 2 hours and poured into saturated saline and extracted with methylene chloride. After washing with water, the methylene chloride layer was dried over anhydrous sodium sulfate. Then, the solvent was removed by distillation and to the residue was added methyl alcohol and the mixture was heated and cooled and crystals which formed were recrystallized form DMF to give 4.5 g of 2-nitro-5-[4-(3,4-dimethoxybenzoyl)-1-piperazinyl]benzaldehyde, m.p. 196°-198° C., yellow crystal.

1. stirringthe mixture was stirred at room temperature for 2 hours
2. additionpoured into saturated saline
3. extractionextracted with methylene chloride
4. washAfter washing with water
5. dry with materialthe methylene chloride layer was dried over anhydrous sodium sulfate
6. customThen, the solvent was removed by distillation and to the residue
7. additionwas added methyl alcohol
8. temperaturethe mixture was heated
9. temperaturecooled
10. customcrystals which formed
11. customwere recrystallized form DMF