反应详情

8-Amino-2-benzylthio[1,2,4]triazolo[1,5-a]pyridine (20.0 g, 0.078 mol), N-chlorosuccinimide (10.4 g, 0.078 mol) and carbon tetrachloride were combined and heated to reflux with stirring for 1 hour. The reaction mixture was cooled, more N-chlorosuccinimide (10.4 g) was added, and the reaction heated to reflux with stirring for another hour. The reaction mixture was then cooled and filtered. The filtrate was concentrated by evaporation under reduced pressure and the residue obtained was purified by column chromatography on silica gel eluting with dichloromethane. The product fractions were concentrated by evaporation under reduced pressure and the residues were combined and mixed with ether. The insoluble solids were collected by filtration and dried to obtain 18.0 g (71 percent of theory) of the title compound as a light tan powder melting at 118°-119° C.

1. temperatureheated
2. temperatureto reflux
3. temperatureThe reaction mixture was cooled
4. temperaturethe reaction heated
5. temperatureto reflux
6. stirringwith stirring for another hour
7. temperatureThe reaction mixture was then cooled
8. filtrationfiltered
9. concentrationThe filtrate was concentrated by evaporation under reduced pressure
10. customthe residue obtained
11. customwas purified by column chromatography on silica gel eluting with dichloromethane
12. concentrationThe product fractions were concentrated by evaporation under reduced pressure
13. additionmixed with ether
14. filtrationThe insoluble solids were collected by filtration
15. customdried