反应详情

Ethyl 4-[(2-chloro-5,6-dimethyl-3-nitropyridin-4-yl)amino]butyrate (86.2 g, 0.276 mol), sodium azide (35.49 g, 0.552 mol), and cerium chloride heptahydrate (50.86 g, 0.138 mol) were triturated in a 9:1 mixture of acetonitrile:water (1012 mL). The reaction mixture was stirred and heated to reflux for 18 hours. The reaction was filtered and the yellow filtrate was concentrated under reduced pressure to yield 90.94 g of crude product. The material was triturated at 95° C. with 360 mL ethyl acetate and filtered. The filtrate produced pale yellow crystals at ambient temperature to afford 64.3 g of ethyl 4-[(5,6-dimethyl-8-nitrotetrazolo[1,5-a]pyridin-7-yl)amino]butyrate as a yellow solid.

1. temperatureheated
2. temperatureto reflux for 18 hours
3. filtrationThe reaction was filtered
4. concentrationthe yellow filtrate was concentrated under reduced pressure
5. customto yield 90.94 g of crude product
6. customThe material was triturated at 95° C. with 360 mL ethyl acetate
7. filtrationfiltered
8. customThe filtrate produced pale yellow crystals at ambient temperature