反应详情

温度

100 °C

A mixture of 2-Cyanopyrimidine (8.0 g, 76 mmol, prepared according to Liebigs Ann.Chem. 2, 1981, 333-341) and Aminoacetaldehyde dimethyl acetal (8 g, 76 mmol) is heated at 100° C. for 4 hours, cooled, and 100 mL of MeOH and 5 mL of concentrated HCl are added. The mixture is heated at reflux with stirring for 30 hours, cooled and evaporated to dryness in vacuo. 50 mL of i-PrOH is added to the residue and the mixture is heated at reflux with stirring for 30 minutes and cooled. The crystals are collected by filtration, washed with ether, and dried to give the title compound. 1H NMR (DMSO): δ 9.08 (d, 2H), 7.87 (s, 2H), 7.75 (t, 1H). LRMS calcd 146, found 147 (MH+).

1. temperaturecooled
2. temperatureThe mixture is heated
3. temperatureat reflux
4. temperaturecooled
5. customevaporated to dryness in vacuo
6. addition50 mL of i-PrOH is added to the residue
7. temperaturethe mixture is heated
8. temperatureat reflux
9. stirringwith stirring for 30 minutes
10. temperaturecooled
11. filtrationThe crystals are collected by filtration
12. washwashed with ether
13. customdried