反应详情

Diethyl 5-[3-(dimethylamino)acryloyl]-1,6-dihydro-6-oxo-2,3-pyridinedicarboxylate (6 g, 0.0178 mol), and p-toluenesulfonic acid (4.5 g, 0.021 mol) in acetic acid (60 mL) are heated at reflux for three hours. The mixture is then evaporated to dryness, neutralized with a saturated NaHCO3 solution and extracted with methylene chloride. The organic solution is dried over Na2SO4, and concentrated to a thick oil, which solidifies after trituration with hexane-ether (4 g, 77%). The product is recrystallized from isopropanol to give a melting point 71°-72° C.

1. temperatureat reflux for three hours
2. customThe mixture is then evaporated to dryness
3. extractionextracted with methylene chloride
4. dry with materialThe organic solution is dried over Na2SO4
5. concentrationconcentrated to a thick oil, which
6. customThe product is recrystallized from isopropanol
7. customto give a melting point 71°-72° C.