反应详情

Under a nitrogen atmosphere, a mixture of ethyl 4-[(2-chloro-5,6-dimethyl-3-nitropyridin-4-yl)amino]butanoate (21.5 g, 68 mmol), sodium azide (8.90 g, 136 mmol), cerium(III) chloride heptahydrate (12.7 g, 34 mmol), and 9:1 acetonitrile:water (250 mL) was heated overnight at reflux. The hot reaction mixture was filtered, and the filter cake was washed with acetonitrile. The filtrate was concentrated under reduced pressure, and the residue was triturated with ethyl acetate:hexanes and isolated by filtration to provide 21.5 g of ethyl 4-[(5,6-dimethyl-8-nitrotetraazolo[1,5-a]pyridin-7-yl)amino]butanoate.

1. temperatureat reflux
2. filtrationThe hot reaction mixture was filtered
3. washthe filter cake was washed with acetonitrile
4. concentrationThe filtrate was concentrated under reduced pressure
5. customthe residue was triturated with ethyl acetate
6. customhexanes and isolated by filtration