摘要
以咪唑为原料,两步硝化得4,5-二硝基咪唑,再在DMF中与硫酸二甲酯反应得目标化合物1-甲基-4,5-二硝基咪唑,采用红外光谱、元素分析、质谱和核磁共振氢谱对其进行了表征。优化了合成工艺,讨论了4,5-二硝基咪唑的硝化机理。实验测得目标产物的总得率为62%,熔点为77℃,最佳反应条件为:温度45～50℃,时间4h,4,5-二硝基咪唑和硫酸二甲酯的摩尔比1:6。在25℃,pH值由4,5-二硝基咪唑(0.63mol·L-1的丙酮溶液)的3.74升到1-甲基-4,5-二硝基咪唑(0.63mol·L-1的丙酮溶液)的6.77,酸性显著降低。
Taking imidazolc as primary substance, 1-methyl-4,5-dinitroimidazole was synthesized in DMF by reaction of methyl sulfate （ （ CH3 ） 2 SO4 ） with 4,5-dlnltroimidazole obtained from nitration. Its structure was eharaeterized by IR, demental analysis, MS and ^1H NMR. The nitration mechanism of 4,5-dinitroimidazole was analyzed. Results show that the yield of 1-methyl-4,5-dinitroimidazole is 62% ,and its melting point is 77 ℃. The optimum parameters are obtained： reaction temperature is 45 -50 ℃ ,and reaction time is 4 h,the molar ratio of 4,5-dinitroimidazole to （ CH3） 2 SO4 is 1 ： 6. The pH value of 4,5-dinitroimidazole （0.63 mol·L^-1 acetone solution） is raised from 3.74 to 6.77 of 1-methyl-4,5-dinitroimidazole （0.63 mol·L^-1 acetone solution）.
出处
《含能材料》
EI
CAS
CSCD
北大核心
2009年第5期531-533,共3页
Chinese Journal of Energetic Materials
