硝解N-叔丁基-3,3-二硝基氮杂环丁烷硝酸盐制备TNAZ

Preparation of TNAZ from Nitrolysis of N-Tert-butyl-3,3-dinitroazetidinium Nitrate

以N-叔丁基-3,3-二硝基氮杂环丁烷硝酸盐(BDNAN)为前体制备1,3,3-三硝基氮杂环丁烷(TNAZ),研究了5种不同的硝解体系,确定了适宜的硝解体系为NH4NO3/Ac2O。探讨了NH4NO3/Ac2O体系的硝解机理,优化了硝解反应条件,确定了最佳反应条件为:n(Ac2O)n(BDNAN)为251,温度为80℃,收率为83.1%,较文献值提高了8.1%。同时初步探讨了TNAZ的热性能和质谱裂解机理,结果表明,TNAZ的熔点较高(99.5℃),分解温度为264.68℃,其四元骨架有一定稳定性。

Taking N-tert-butyl-3,3-dinitroazetidinium nitrate（BDNAN）as precursor,1,3,3-trinitroazetidine（TNAZ）was synthesized by five different nitrolysis systems.The optimal nitrolysis system was NH4NO3/Ac2O.At the same time,the reaction conditions were optimized,and the optimal reaction conditions are as follows：n（Ac2O）n（BDNAN）=251,reaction temperature is 80 ℃ and yield is 83.1%.The thermal characteristics and the split mechanism of TNAZ were studied.Results show that TNAZ having a stable four-membered ring skeleton melts at 99.5 ℃ with decomposition at 264.68 ℃.