反应详情

温度

100 °C

In 20 ml of N,N-dimethylformamide was dissolved 1 g of dimethyl 4-[2-(4-aminobutoxy)-5-nitrophenyl]-2,6-dimethyl-1,4-dihydropyridine-3,5-dicarboxylate. The solution was heated at 100° C. for 1.5 hours. The reaction solution was carefully poured onto 500 ml of ice water. The precipated oily substance was extracted with ethyl acetate. After drying over anhydrous sodium sulfate, the solvent was removed by distillation under reduced pressure. The obtained residue was subjected to silica gel column chromatography and eluted by chlorform:methanol (96:4 v/v). The obtained crude crystals were recrystallized form ethanol to give 1.2 g of dimethyl 4-[2-[4-(3-phenoxypropylamino)butoxy]-5-nitrophenyl]-2,6-dimethyl-1,4-dihydropyridine-3,5-dicarboxylate. This compound has the following physicochemical properties.

1. extractionThe precipated oily substance was extracted with ethyl acetate
2. dry with materialAfter drying over anhydrous sodium sulfate
3. customthe solvent was removed by distillation under reduced pressure
4. washeluted by chlorform:methanol (96:4 v/v)
5. customThe obtained crude crystals
6. customwere recrystallized form ethanol