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出 处:《高校化学工程学报》2013年第2期248-253,共6页Journal of Chemical Engineering of Chinese Universities
摘 要:研究了三种合成2,6-二氨基-3,5-二硝基吡嗪-1-氧化物(LLM-105)的新方法。此三种方法均以N-亚硝基二(氰甲基)胺为起始原料,经过环合制备2,6-二氨基吡嗪,再分别经硝化、氮氧化;氮氧化、硝化;乙酰化、氮氧化、硝化三种方法得到LLM-105,通过对硝化反应、氮氧化反应条件以及目标产物总收率和纯度分析,发现2,6-二氨基吡嗪经乙酰化、氮氧化、硝化反应合成路线最佳,LLM-105的收率可达45.8%,纯度大于99%。测试了LLM-105的爆速、爆压、DSC及落锤感度,同1,3,5-三氨基-2,4,6-三硝基苯(TATB)进行了对比,发现其性能优于TATB。用1H-NMR、IR、MS对LLM-105及其中间体结构进行了表征。Three new synthetic routes of2,6-diamino-3,5-dinitropyrazine-1-oxide (LLM-105) were described. 2,6-Diaminopyrazine, as the precursor of LLM-105, was synthesized via cyclization with N-nitrosobis(cyanomethyl) amine as the starting material, and then LLM-105 was synthesized via three different routes: nitration and N-oxidation for the first route, N-oxidation and nitration for the second route, and acetylation, N-oxidation and nitration for the third route. Through the comparisons of the reaction conditions of nitration and N-oxidation, the total yield and purity of the target product of the three different routes, it was found that the optimum reaction route is the route with acetylation, N-oxidation and nitration; when using it, the yield of LLM-105 is 45.8%, and purity is over 99%. Detonation velocity, detonation pressure, DSC and sensitivities of impact for LLM-105 were measured and the results show that the capabilities of LLM-105 are greater than that of TATB. The structures of the intermediates and LLM-105 were characterized by 1H-NMR, IR, MS spectra, respectively.
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