反应详情

A mixture of amine (1f) (0.403 g, 1.4 mmol), 2-vinyl-quinoxaline (b), (0.22 g, 1.4 mmol), acetic acid (0.1 ml) and ethanol (5.2 ml) was heated under reflux for 6 hours. The mixture was then made basic with aqueous sodium hydroxide and extracted with ethyl acetate. The organic phase was washed with water, dried over magnesium sulfate and concentrated. The residue was chromatographed on silica gel eluting with dichloromethane-methanol (99-1). After evaporation the residue was triturated with a small amount of ethyl acetate and crystallised. The solid was collected by filtration and dried to give the title compound (80 mg) mp.: 170° C.

1. temperaturewas heated
2. temperatureunder reflux for 6 hours
3. extractionextracted with ethyl acetate
4. washThe organic phase was washed with water
5. dry with materialdried over magnesium sulfate
6. concentrationconcentrated
7. customThe residue was chromatographed on silica gel eluting with dichloromethane-methanol (99-1)
8. customAfter evaporation the residue
9. customwas triturated with a small amount of ethyl acetate
10. customcrystallised
11. filtrationThe solid was collected by filtration
12. customdried