摘要
以4-硝基咪唑为原料，经硝化、热重排、甲基化等反应合成1-甲基-2，4，5-三硝基咪唑（MTNI），总收率19．4％，纯度〉98％，经红外光谱、核磁共振、元素分析等方法表征其结构。研究了反应温度、反应时间等因素对1-甲基-2，4-二硝基咪唑（MDNI）合成及收率的影响，得到了较优的工艺条件：n（2，4-二硝基咪唑）：n（碘甲烷）-5：9，反应温度40-45℃，反应时间8h。对硝化反应条件进行了研究，确定了适宜反应时间为1h，反应温度为95℃。
Taking 4-nitroimidazole as primary substance, 1-methyl-2,4,5-trinitroimidazole （MTNI） was synthesized via nitration, thermal rearrangement and methylation.The overall yield of MTNI was 19.4%.The purity of MTNI was more than 98%.The structures were characterized by IR, 1H NMR and elemental analysis. The effects of reaction temperature, reaction time on the synthesis and yield were investigated. The synthestic condition was optimized by the orthogonal experiment. The optimum parameters are as follows： n （2,4-DNI）：n （CH3I）=5：9, reaction temperature 40-45℃ and reaction time 8 h.Through an investigation of nitration the conditions, the optimal reaction time and temperature wasconsidered to be 1 h and 95℃ respectively.
出处
《精细化工中间体》
CAS
2008年第5期30-33,共4页
Fine Chemical Intermediates
