反应详情

To a cooled, stirred mixture of 2 g. of 1,2,4-triazole-3-carboxamide and 5.4 g. salicyloyl chloride in 125 ml. of anhydrous diethyl ether is added rapidly 2.75 g. of triethylamine. The cooling bath is removed and the mixture is stirred at room temperature for 22 hours. The mixture is filtered and the solid is collected and washed successively with diethyl ether, cold water, diethyl ether and dried in vacuo for 4 hours. The solid is extracted with hot, dry acetonitrile. The filtrate is reduced to about half volume by evaporation in vacuo over a warm water bath and filtered to separate a small amount of solid which separates for 2 hours. Further evaporation of the resulting filtrate to a very small volume results in the separation of a solid which is collected, washed with acetonitrile and dried yielding 210 m.p. 125°-135° C. (dec.).

1. additionmixture of 2 g
2. customThe cooling bath is removed
3. stirringthe mixture is stirred at room temperature for 22 hours
4. filtrationThe mixture is filtered
5. customthe solid is collected
6. washwashed successively with diethyl ether, cold water, diethyl ether
7. customdried in vacuo for 4 hours
8. extractionThe solid is extracted with hot, dry acetonitrile
9. customThe filtrate is reduced to about half volume by evaporation in vacuo over a warm water bath
10. filtrationfiltered
11. customto separate a small amount of solid which
12. customFurther evaporation of the resulting filtrate to a very small volume
13. customresults in the separation of a solid which
14. customis collected
15. washwashed with acetonitrile
16. customdried
17. customyielding 210 m