反应详情

Sodium (3.11 g, 135 mmol) was added to 250 ml of absolute ethanol in a 500 ml round bottom flask and allowed to react under nitrogen. N-(2,6-dichloro-3-methylphenyl)-5-amino-1,2,4-triazole-3-sulfonamide (14.5 g, 45 mmol) and then dimethyl malonate (11.9 g, 90 mmol) were added and the mixture heated at reflux with stirring for about three days. The mixture was then cooled with an ice bath and filtered to collect the solids. These were washed with hexane and dissolved in about 75 ml of cold water and the resulting solution was acidified to about pH 2 with conc. hydrochloric acid. The precipitate that formed was collected by filtration and dried to obtain 13.55 g (77.1 percent of theory) of the title compound as a white powder, which decomposes above 200° C. This was shown to be the title compound by NMR.

1. customto react under nitrogen
2. temperaturethe mixture heated
3. temperatureat reflux
4. temperatureThe mixture was then cooled with an ice bath
5. filtrationfiltered
6. customto collect the solids
7. washThese were washed with hexane
8. dissolutiondissolved in about 75 ml of cold water
9. customThe precipitate that formed
10. filtrationwas collected by filtration
11. customdried