反应详情

Diethyl 1-amino-1,2-ethylenedicarboxylate (1.0 g) and acrolein monomer (0.39 g) are dissolved in n-butanol (10 ml), and thereto is added p-toluenesulfonic acid (20 mg). The mixture is refluxed for 10 hours, and thereto is added additional acrolein monomer (0.1 g), and the mixture is refluxed for 5 hours (the degree of reaction of aminodiester is 91%). After distilling off the solvent, the residue is distilled under reduced pressure to give diethyl pyridine-2,3-dicarboxylate (0.86 g, 72.3%). The product has a boiling point of 135°-145° C. (3 Torr) and a purity of 96.4% by gas chromatographic analysis.

1. temperatureThe mixture is refluxed for 10 hours
2. temperaturethe mixture is refluxed for 5 hours (
3. distillationAfter distilling off the solvent
4. distillationthe residue is distilled under reduced pressure