Synthesis Of4H-1,2,4-triazol-4-amine

Based on the summary of ethyl formate、1,2-Diformylhydrazine、4H-1,2,4-Triazol-4-amine, the synthesis of ethyl formate、1,2-Diformylhyd-razine,4H-1,2,4-Triazol-4-amine are studied, we got the suitable technolog-ical conditions via analysis of the influencing factors of reaction yield and their structure was confirmed via analysis of IR、1NMR、13CNMR、MS. At the same time, we introduced its applications and the vision of its future.Ethyl is synthesized with formic acid and absolute ethyl alcohol as the material, KHSO4as the catalyst. The effects of the different catalyst and do-sage of these catalysts, the different ratio of anhydrous ethanol and formic a-cid, different temperature on the yield of ethyl formate were investigated. The optimized synthesis parameters are as follows:The consumption of for-mic acid and absolute ethyl alcohol are11mL and30mL respectively, the a-mount of catalyst is1g, temperature of the reaction is65℃, time of the r-eaction is2h. The yield is85%, the catalyst can be recycled when necessa-ry.1,2-Diformylhydrazine is synthesized with ethyl formate, which is syn-thesized in my laboratory, and hydrazine hydrate as the material, formic ac-id as the catalyst. The effects of the different ratio of ethyl formate and hy-drazine hydrate, different reaction time, different temperature on the yield o-f1,2-Diformylhydrazine were investigated. The optimized synthesis para-meters are as follows:The consumption of ethyl formate20mL and hydrazi-ne10mL, the amount of formic acid is15mL, temperature of the reaction is70℃, under atmospheric pressure2h and then vacuum for1h. The yield is85%.4H-1,2,4-Triazol-4-amine is synthesized with1,2-Diformylhydrazine, which is synthesized in my laboratory, and hydrazine hydrate as the materia-1, polyphosphoric acid as the catalyst. The effect of the different ratio of1,2-Diformylhydrazine and hydrazine hydrate, different reaction time, diff- erent temperature on the yield of4H-1,2,4-Triazol-4-amine were investigat-ed. The optimized synthesis parameters are as follows:The consumption of1,2-Diformylhydrazine and hydrazine hydrate12.1g and10mL respectively, the amount of catalyst is3g, temperature of the reaction is150℃, under atmospheric pressure3h and then vacuum for1h. The yield is70.5%. In order to get more purer4H-1,2,4-Triazol-4-amine, the method of isopropyl alcohol recrystallization is used.