反应详情

Sodium methoxide (0.54 g) and 4-cyanopyridine (10.4 g) were combined in anhydrous methanol (100 ml) and stirred at room temperature for 18 h, under a nitrogen atmosphere. Ammonium chloride (5.99 g) was then added, and the mixture heated to reflux for 4 h, under a calcium chloride guard tube. The reaction was cooled, evaporated under reduced pressure, re-suspended in ethanol (120 ml) and heated to reflux for another 15 min. The resultant white precipitate was filtered off, dried, then triturated with ice-cold water and dried under vacuum at 40° C. to yield the title compound as a white solid (7.44 g, 47%). Two further crops were obtained through concentration of the ethanol filtrate (total yield 12.1 g, 77%)

1. temperaturethe mixture heated
2. temperatureto reflux for 4 h, under a calcium chloride guard tube
3. temperatureThe reaction was cooled
4. customevaporated under reduced pressure
5. temperatureheated
6. temperatureto reflux for another 15 min
7. filtrationThe resultant white precipitate was filtered off
8. customdried
9. customtriturated with ice-cold water
10. customdried under vacuum at 40° C.