反应详情

6-Cyano-pyrido[3,4-d]pyrimidin-4-one (0.3 g) in diglyme (2 ml) was treated with tributyl tin azide (0.49 g) at reflux under N2 for 15 hours. The cooled mixture was partitioned between ethyl acetate and water and the aqueous phase extracted further with ethyl acetate. The aqueous phase was concentrated in vacuo, the residue taken up in methanol and inorganics removed by filtration. Subsequent concentration gave the title compound (1.4 g) as a beige solid; δH [2H6]DMSO 8.96 (1H,s), 8.50 (1H,s), 8.27 (1H,s); m/z (M+1+)216.

1. temperatureat reflux under N2 for 15 hours
2. customThe cooled mixture was partitioned between ethyl acetate and water
3. extractionthe aqueous phase extracted further with ethyl acetate
4. concentrationThe aqueous phase was concentrated in vacuo
5. custominorganics removed by filtration
6. concentrationSubsequent concentration