反应详情

温度

80 °C

2-Nitro-5-[4-(3,4-dimethoxybenzoyl)-1-piperazinyl]benzaldehyde (4 g) was dissolved in 20 ml of pyridine followed by adding 2.1 g of malonic acid and 0.4 ml of piperidine, and the mixture was stirred at 80° C. for 4 hours. After evaporating pyridine and piperidine the reaction mixture was poured in a dilute aqueous hydrogen chloride solution and extracted with methylene chloride. After washing the methylene chloride layer with water the solvent was distilled off and methanol was added to the residue. After cooling, crystals which formed were collected by filtration to give 3.7 g of 2-nitro-5-[4-(3,4-dimethoxybenzoyl)-1-piperazinyl]-cinnamic acid, m.p. 197°-202° C.

1. customAfter evaporating pyridine and piperidine the reaction mixture
2. additionwas poured in a dilute aqueous hydrogen chloride solution
3. extractionextracted with methylene chloride
4. washAfter washing the methylene chloride layer with water the solvent
5. distillationwas distilled off
6. additionmethanol was added to the residue
7. temperatureAfter cooling
8. customcrystals which formed
9. filtrationwere collected by filtration