2,4,6-三硝基-3,5-二氨基-N-(1,2,4-三唑-4)-苯胺的合成

Synthesis of 2,4,6-Trinitro-3,5-diamino-N-(1,2,4-triazole-4)-aniline

以2,4,6-三硝基氯苯为原料,先与甲胺醇溶液反应得到1-甲氨基-2,4,6-三硝基苯,再经硝硫混酸硝化得到2,4,6-三硝基苯甲硝铵,最后以二甲亚砜为溶剂,强碱甲醇钠为活化剂,与4-氨基-1,2,4-三氮唑反应得到2,4,6-三硝基-3,5-二氨基-N-(1,2,4-三唑-4)-苯胺,总收率达80.18%,并通过1H NM R、M S、IR对中间体和产物进行了表征。结合反应机理,讨论了影响2,4,6-三硝基-3,5-二氨基-N-(1,2,4-三唑-4)-苯胺合成的关键因素,对其进行DSC和T G测试,结果表明两个热分解峰温分别为210℃和328℃,在200℃以下未出现明显的质量损失过程,升温至500℃分解残渣为38.89%,其热稳定性良好。

2,4,6-Trinitro-3,5-diamino-N-（1,2,4-triazole-4）-aniline was synthesized using 2,4,6-trinitrochlorobenzene as the start material which firstly reacted with methylamine alcohol solution, then reacted with sulfuric acid and nitric acid, and finally reacted with 4-amino-1,2,4-triazole（ATA） and methanol sodium. The total yield is 80.18%. The target compound and its intermediates were identified by IR, MS and 1H NMR. The main affecting factors of the reactions were discussed based on reaction mechanism. The results of the DSC test show that the two thermal decomposition peak temperature are respectively 210 ℃ and 328 ℃. The results of the TG test show that there is not any obvious quality loss process below 200 ℃, and the residual decomposition is 38.89% when the temperature is up to 500 ℃, indicating the final compoud has good thermal stability.