反应详情

温度

60 °C

To a solution of ethyl 3-(dimethylamino)-2-(2-fluoro-5-iodobenzoyl)acrylate (Intermediate 24, 1 g, 2.56 mmol) dissolved in THF (5.5 mL) was added 2-(1-methylpiperidin-4-yl-ethanamine (0.406 mL, 2.56 mmol). The reaction mixture was stirred at 60° C. for 2 h. Potassium carbonate was added (1.06 g, 7.67 mmol), and the reaction was stirred for 18 h and cooled down to room temperature. The reaction was quenched with 1 N HCl and partitioned between dichloromethane (10 mL) and water (20 mL). The aqueous layer was extracted with dichloromethane (2×10 mL), and the organics were dried over sodium sulfate and concentrated to give ethyl 6-iodo-1-(2-(1-methylpiperidin-4-yl)ethyl)-4-oxo-1,4-dihydroquinoline-3-carboxylate as a light yellow solid (1.08 g, 90%).

1. stirringthe reaction was stirred for 18 h
2. temperaturecooled down to room temperature
3. customThe reaction was quenched with 1 N HCl
4. custompartitioned between dichloromethane (10 mL) and water (20 mL)
5. extractionThe aqueous layer was extracted with dichloromethane (2×10 mL)
6. dry with materialthe organics were dried over sodium sulfate
7. concentrationconcentrated