1-氨基-1,2,3-三唑的合成

Synthesis of 1-Amino-1,2,3-triazole

以乙二醛、水合肼为起始原料反应得到乙二醛双腙,经活性MnO2催化氧化成环制得1-氨基-1,2,3-三唑,采用红外光谱、元素分析、核磁共振和质谱对其进行了表征。就中间体乙二醛双腙重结晶纯化、氧化剂MnO2用量优化、产物纯化方法等几方面进行了改进,优化了1-氨基-1,2,3-三唑的合成工艺,得到了高纯(96%)的1-氨基-1,2,3-三唑。并对1-氨基-1,2,3-三唑的成环和分解机理进行了讨论。

A preparation method of 1-amino-1,2,3-triazole was developed. The glyoxal bishydrazone was synthesized from glyoxal and aqueous hydrazine, and then glyoxal bishydrazone was oxidated with activated manganese dioxide to give 1-amino-1,2,3-triazole. The structure of 1-amino-1,2,3-triazole was confirmed by IR, elemental analysis, NMR and MS. Results show that 1-amino-1,2,3-triazole with high purity （96%） can be optimally got by crystallization from acetonitrile. The optimal amount of manganese dioxide is 2.8 N to the amount of glyoxal bishydrazone, and the reaction can be achieved within 2.5 h with the yield of 78.30%. In addition, the reaction mechanisms of decomposition and synthesis of 1-amino-1,2,3-triazole were discussed.