反应详情

Fifty-five g of 1,3-dimethyl-4-nitro-5-chloropyrazole was dissolved in 400 ml acetonitrile and 17.45 g potassium cyanide added, followed by 0.5 g potassium iodide and 5 ml DMF. The mixture was refluxed for 22 hours, then cooled, and filtered. The filtrate was concentrated under reduced pressure, then added to stirred water. The resulting percipitate was collected, dried, and recyrstallized in isopropanol. mp, 85°-87° C. A second recrystallization again in ethanol gave the product having increased purity, mp 96°-98° C.

1. temperatureThe mixture was refluxed for 22 hours
2. temperaturecooled
3. filtrationfiltered
4. concentrationThe filtrate was concentrated under reduced pressure
5. additionadded
6. customThe resulting percipitate was collected
7. customdried
8. custommp, 85°-87° C
9. customA second recrystallization again in ethanol
10. customgave the product
11. temperaturehaving increased purity, mp 96°-98° C.