反应详情

A solution of 32.2 g (0.10 mol) of N-(2,6-dichloro-3-methylphenyl)-5-amino-1,2,4-triazole-3-sulfonamide and 14 ml (0.11 mol) of ethyl acetoacetate in 500 ml of methanol containing 1 ml of 12N hydrochloric acid was heated to reflux with stirring for about 18 hours. The solid present was collected by filtration and the filtrate was heated to reflux for another day. The mixture obtained was cooled in an ice bath and the solid present was collected by filtration. The filtrate was concentrated to about 200 ml by evaporation of methanol and heated to reflux overnight. The mixture obtained was filtered to collect the solid present. The filtrate was concentrated to about 150 ml, treated with about 2 ml of ethyl acetoacetate, and heated at reflux for about 3 days. The solids present were collected by filtration and dried to obtain 6.4 g, 10.0 g, 8.2 g and 11.1 g crops of the title compound for a total of 35.7 g (92 percent of theory). The first obtained crop melted at 346°-7° C. with decomposition.

1. temperatureto reflux
2. filtrationThe solid present was collected by filtration
3. temperaturethe filtrate was heated
4. temperatureto reflux for another day
5. customThe mixture obtained
6. temperaturewas cooled in an ice bath
7. filtrationthe solid present was collected by filtration
8. concentrationThe filtrate was concentrated to about 200 ml by evaporation of methanol
9. temperatureheated
10. temperatureto reflux overnight
11. customThe mixture obtained
12. filtrationwas filtered
13. customto collect the solid present
14. concentrationThe filtrate was concentrated to about 150 ml
15. additiontreated with about 2 ml of ethyl acetoacetate
16. temperatureheated
17. temperatureat reflux for about 3 days
18. filtrationThe solids present were collected by filtration
19. customdried