1-氨基-3-甲基-1,2,3-三唑硝酸盐的合成与表征

以乙二醛和水合肼为起始原料,经加成-消除、环化甲基化、置换反应得到1-氨基-3-甲基-1,2,3-三唑硝酸盐(1-AMTN),总收率71.8%(以乙二醛计),采用核磁(NMR)、红外(IR)、质谱(MS)和元素分析对产物进行了表征。预测了1-AMTN的性能:密度为1.63 g.cm-3,生成焓84 kJ.mol-1,爆速8115 m.s-1。研究了溶剂、温度、物料比对产物得率的影响,确定了环化甲基化的最佳反应条件:溶剂为乙腈,反应温度20℃,乙二腙与碘甲烷的物料比1∶5,环化甲基化收率为86.7%。对活性二氧化锰进行了回收利用并对其机理进行了探讨。

Synthesis and Characterization of 1-Amino-3-methyl-1,2,3-triazolium Nitrate

1-Amino-3-methyl-1,2,3-triazolium nitrate(1-AMTN) was synthesized using glyoxal and hydrazine hydrate as starting materials in three steps,i.e.addition-elimination,cyclization,methylation and replacement reaction.The overall yield is 71.8%(based on glyoxal).The structure of products was confirmed by IR,MS,NMR and elemental analysis.The properties of 1-AMTN were estimated: density 1.63 g·cm-3,enthalpy of formation 84 kJ·mol-1 and detonation velocity 8115 m·s-1.The key factors of cyclization and methylation were studied and the optimal reaction conditions were confirmed: medium acetonitrile,20 ℃,and the ratio of glyoxal bishydrazone and methyl Iodide 1∶5.The overall yield of cyclization and methylation is 86.7%.In addition,actived manganese oxide was recycled and its mechanism was also discussed.