反应详情

温度

125 °C

To a mixture of PPA (10 g) and acetoacetamide triethylamine (2.02 g, 20 mmol) was added benzylacetone (5.92 g, 5.98 mL, 40 mmol). The resulting mixture was heated at 125° C. for 3 hours. The brown mixture was poured onto crushed ice and neutralized with solid NaHCO3. The mixture was filtered to give a yellow solid, which was purified by flash column (silica, 10% MeOH/DCM) to give the pyridinone (2.29 g, 53.8%) as a yellow solid. 1H NMR (CDCl3) δ 2.07 (s, 3H), 2.37 (s, 3H), 3.81 (s, 2H), 6.38 (s, 1H), 7.00-7.40 (m, 5H); MS (CI) m/z 214.1 (MH+).

1. additionThe brown mixture was poured
2. customonto crushed ice
3. filtrationThe mixture was filtered
4. customto give a yellow solid, which
5. customwas purified by flash column (silica, 10% MeOH/DCM)