反应详情

To a suitably equipped reaction vessel was charged 116 g (1.0 mole) of 5-amino-3-mercapto-1,2,4-triazole and 500 ml of pyridine. A total of 147.5 g (1.05 mole) of benzoyl chloride was added with vigorous stirring over 25 minutes, during which time the temperature rose from 24° to 59° C. The mobile, pale yellow slurry obtained was heated at reflux with stirring. The solid material dissolved and then, after about 40 additional minutes, a white solid began separating. An additional 200 ml of pyridine was added to aid mixing and the reaction was continued at 117°-122° for a total of 7 hours. The thick, white slurry obtained was filtered, washed with water and with methylene chloride, and dried to obtain 186 g (84 percent of theory) of the title compound, m.p. 311°-312° (dec.).

1. customTo a suitably equipped reaction vessel
2. customrose from 24° to 59° C
3. customThe mobile, pale yellow slurry obtained
4. temperaturewas heated
5. temperatureat reflux
6. stirringwith stirring
7. dissolutionThe solid material dissolved
8. customafter about 40 additional minutes, a white solid began separating
9. additionAn additional 200 ml of pyridine was added to aid
10. additionmixing
11. customwas continued at 117°-122° for a total of 7 hours
12. customThe thick, white slurry obtained
13. filtrationwas filtered
14. washwashed with water and with methylene chloride
15. customdried