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发明公开
CN108047146A 含能化合物1,2,3-三氮唑-4,5-双偕二硝基二钾盐及其制备方法 有权

含能化合物1,2,3-三氮唑-4,5-双偕二硝基二钾盐及其制备方法
摘要：
本发明公开了含能化合物1,2,3‑三氮唑‑4,5‑双偕二硝基二钾盐。本发明还公开了含能化合物1,2,3‑三氮唑‑4,5‑双偕二硝基二钾盐的制备方法，包括以下步骤：第一步，0℃下将1,2,3‑三氮唑‑4,5‑二氯肟的氯仿溶液加入到100％硝酸、三氟乙酸酐和三氟乙酸的混合溶液中，然后恢复至25℃进行充分反应，随后倒入冰水淬灭，氯仿萃取旋蒸至油状物，将油状物经色谱柱分离得到中间体1,2,3‑三氮唑‑4,5‑双偕二硝基氯；第二步，将中间体溶于无水甲醇，加入碘化钾的无水甲醇溶液，常温反应后过滤得到目标产物1,2,3‑三氮唑‑4,5‑双偕二硝基二钾盐。本发明的三氟乙酸酐/三氟乙酸/硝酸体系有利于本发明的目标化合物实现。
摘要（英）：

The invention discloses an energetic compound 1,2,3-triazole-4,5-bisgem-dinitro dipotassium salt. The invention further discloses a preparation method of the energetic compound 1,2,3-triazole-4,5-bisgem-dinitro dipotassium salt. The preparation method comprises the following steps: 1, adding a chloroform solution of 1,2,3-triazole-4,5-dichlorooxime into a mixed solution of 100% of nitric acid, trifluoroacetic anhydride and trifluoroacetic acid at a temperature of 0 DEG C, restoring to a temperature of 25 DEG C to be fully reacted, pouring ice water for quenching, extracting with chloroform andperforming rotary evaporator to obtain an oily matter, and performing chromatographic column separation on the oily matter to obtain an intermediate 1,2,3-triazole-4,5-bisgem-dinitro chloride; 2, dissolving the intermediate into absolute methanol, adding an absolute methanol solution of potassium iodide, reacting at a normal temperature, and filtering, thereby obtaining the target product 1,2,3-triazole-4,5-bisgem-dinitro dipotassium salt. According to the method disclosed by the invention, the trifluoroacetic anhydride/trifluoroacetic acid/nitric acid system contributes to realizing the target compound in the invention.

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