反应详情

A mixture of N4-(1-ethyl-propyl)-6-methyl-N2-(2,4,6-trimethyl-phenyl)-pyridine-2,3,4-triamine (250 mg, 0.77 mmol), trimethyl orthoformate (0.081 g, 0.766 mmol), p-toluenesulfonic acid monohydrate (0.01 g) in benzene was heated at reflux using Dean-Stark apparatus for 24 hours. Benzene was removed and toluene was added and an excess of trimethyl orthoformate (0.084 ml) was added to the reaction mixture. The mixture was heated at reflux overnight. The mixture was quenched with water, sat. NaHCO3, extracted with ethyl acetate. The organic layer was separated, dried (MgSO4) and concentrated to dryness. After purification, the title compound was isolated as a white crystal, mp 78–80° C.

1. temperaturewas heated
2. temperatureat reflux
3. customfor 24 hours
4. customBenzene was removed
5. additiontoluene was added
6. additionan excess of trimethyl orthoformate (0.084 ml) was added to the reaction mixture
7. temperatureThe mixture was heated
8. temperatureat reflux overnight
9. customThe mixture was quenched with water, sat. NaHCO3
10. extractionextracted with ethyl acetate
11. customThe organic layer was separated
12. dry with materialdried (MgSO4)
13. concentrationconcentrated to dryness
14. customAfter purification