反应详情

Tin(II) chloride dihydrate (346.3 g, 1.54 mol) was added to a solution of 2,3,6,7-tetrachloro-5-nitroquinoxaline (96.2 g, 0.31 mol) in ethyl acetate (1.8 L). The mixture was heated under reflux for 4 hours, cooled and poured cautiously into an excess of aqueous saturated sodium bicarbonate solution. The mixture was filtered through CELITE (trade mark), washing well with ethyl acetate. The filter cake was macerated with further ethyl acetate and the solid material filtered off. The combined ethyl acetate phases were dried (MgSO4) and concentrated under reduced pressure to give 5-amino-2,3,6,7-tetrachloroquinoxaline (73.4 g, 84%) as a yellow solid.

1. temperatureThe mixture was heated
2. temperatureunder reflux for 4 hours
3. temperaturecooled
4. filtrationThe mixture was filtered through CELITE (trade mark)
5. washwashing well with ethyl acetate
6. filtrationthe solid material filtered off
7. dry with materialThe combined ethyl acetate phases were dried (MgSO4)
8. concentrationconcentrated under reduced pressure