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以氨基胍碳酸氢盐与丙二酸为原料,经缩合–环化反应、重氮化–取代反应和硝化反应合成出5–硝基–3–三硝甲基–1H–1,2,4–三唑。用红外光谱、核磁共振、元素分析对其结构进行了表征。确定了最佳硝化反应体系:5–硝基–1H–1,2,4–三唑–3–乙酸为硝化反应前体,硝硫混酸(V(w为的98%浓硫酸)∶V(发烟硝酸)=1.2∶1)为硝化剂。采用密度泛函理论(DFT)中B3LYP方法在6–31G(d,p)基组水平下对5–硝基–3–三硝甲基–1H–1,2,4–三唑进行了全构型优化,并在优化构型基础上进行了自然键轨道(NBO)分析。差示扫描量热法(DSC)分析结果表明,10℃/min升温速率下,5–硝基–3–三硝甲基–1H–1,2,4–三唑的分解温度为135℃。
Aminoguanidine bicarbonate and malonic acid were used as starting materials to synthesize 5-nitro-3-trinitro-1H-1,2,4-oxadiazole by condensation-cyclization reaction, diazotization-substitution reaction and nitration reaction - triazole. Its structure was characterized by IR, 1H NMR and elemental analysis. The best nitration reaction system was determined: 5-Nitro-1H-1,2,4-triazole-3-acetic acid was the precursor of nitration reaction, Fuming nitric acid) = 1.2: 1) as a nitrating agent. Nitro-3-trinitro-1H-1,2,4-triazole was carried out using the B3LYP method in density functional theory (DFT) at the 6-31G (d, p) Configuration optimization, and based on the optimized configuration of the natural bond orbital (NBO) analysis. Differential scanning calorimetry (DSC) analysis showed that the decomposition temperature of 5-nitro-3-trinitro-1H-1,2,4-triazole was 135 ° C at a heating rate of 10 ° C / min.