反应详情

温度

90 °C

Ethyl 2-(5-bromo-2-fluoronicotinoyl)-3-(dimethylamino)acrylate (Intermediate 3, 2.0 g, 5.79 mmol), (S)-tert-butyl 3-aminopiperidine-1-carboxylate (1.160 g, 5.79 mmol), and potassium carbonate (2.042 g, 7.38 mmol) were combined in DMF (10.0 mL). The reaction mixture was heated at 90° C. for 2 h. The reaction mixture was cooled to 0° C. and 1N HCl was slowly added until pH was 5. The resulting precipitate was collected by filtration, washed with water and dried overnight to yield a light yellow solid (2.10 g, 75%).

1. temperatureThe reaction mixture was cooled to 0° C.
2. filtrationThe resulting precipitate was collected by filtration
3. washwashed with water
4. customdried overnight