摘要
以咪唑为原料,通过两步硝化制得1,4-二硝基咪唑,然后在氯苯中热重排得2,4-二硝基咪唑,将2,4-二硝基咪唑进一步硝化并制得2,4,5-三硝基咪唑的钾盐,最后将钾盐甲基化,得到1-甲基-2,4,5-三硝基咪唑。采用红外光谱、元素分析、核磁的方法对其结构进行表征。用DSC进行了热分解研究。同时优化了2,4-二硝基咪唑的重排工艺:反应温度为120℃~125℃,反应时间为4h,1,4-二硝基咪唑和氯苯的物质的量比为1:30。对2,4,5-三硝基咪唑不稳定性进行了分析。
1-methy1-2,4,5-trinitroimidazole (MTNI)is an important polynitro imidazole compoundd.It was synthesized with imidazole as primary substance,by nitrateion obtaining 1,4-dinitroimidazole,and then thermal rearrangement in ehlorobenzene,obtaining 2,4-dinitroimidazole.Natration 2,4-dinitroimidazole and make it become Potassium 2,4,5-trinitroimidazolate.The last,Potassium 2,4,5-trinitroimidazolate was methylated,obtaining 1- methy1-2,4,5-trinitroimidazole.Its structure was characterized by IR elemental analysis and H1NMR.Thermal decomposition of 1-methyl-2,4,5-trinitroimidazole was studied by DSC.Meanwhile,investingating thermal rearrangement, The optimum parameters were as follows;n (1,4-dinitroimidazole)/n (chlorobenzene)=1:30,reaction temperature 120℃-125℃,reaction time 4h. And explain why 2,4,5-trinitroimidazole was unstable.
出处
《天津化工》
CAS
2009年第4期20-22,42,共4页
Tianjin Chemical Industry