反应详情

温度

65 °C

To a suspension of sodium selenide (0.9 g, 7.2 mmol, prepared from 0.75 g of selenium as described above) in DMF (7 mL) was added a solution of 2-chloropyridine-3-carbonitrile (1 g, 7.2 mmol) in DMF (3 mL) at rt for 5 min and stirred the mixture at 60-70° C. for 2 h. Then chloroacetonitrile (0.46 mL, 7.22 mmol) was added dropwise to the reaction mixture and again stirred at 60-70° C. for 2 h. Then, a solution of sodium methoxide (0.39 g, 7.2 mmol) in methanol (7 mL) was added dropwise and stifling was continued for 1 h at the same temperature. The mixture was allowed to room temperature (rt) and poured into cold water and stirred for 15 min. The precipitated solid was filtered, washed with water and dried to give the product as a yellow color solid (1.3 g, 81%), mp 208-210° C. 1H NMR (400 MHz, DMSO-d6): δ 8.68 (1H, d, J=4.4 Hz, H-6), 8.47 (1H, d, J=8.4 Hz, H-4), 7.55 (1H, dd, J=8.0, 4.8 Hz, H-5), 7.24 (2H, s, —NH2).

1. stirringagain stirred at 60-70° C. for 2 h
2. waitstifling was continued for 1 h at the same temperature
3. customwas allowed to room temperature
4. custom(rt)
5. stirringstirred for 15 min
6. filtrationThe precipitated solid was filtered
7. washwashed with water
8. customdried