反应详情

温度

105 °C

To a solution of 4-methoxy-2-oxo-1,2-dihydro-pyridine-3-carbonitrile (19.81 g, 131.98 mmol) in acetonitrile (520 ml) were added intermediate 1 (34.36 g, 171.57 mmol) and potassium carbonate (56.73 g, 410.3 mmol) and the mixture was heated at 105° C. for 12 hours. The mixture was cooled to room temperature and the solid was filtered off The filtrate was evaporated till dryness. The crude product was purified by column chromatography (silica gel; DCM to DCM/EtOAc up to 20% as eluent). The desired fractions were collected and evaporated in vacuo to yield intermediate 3 (13.18 g, 46%).

1. temperatureThe mixture was cooled to room temperature
2. filtrationthe solid was filtered off The filtrate
3. customwas evaporated till dryness
4. customThe crude product was purified by column chromatography (silica gel; DCM to DCM/EtOAc up to 20% as eluent)
5. customThe desired fractions were collected
6. customevaporated in vacuo