1,3,5,7-四硝基-1,3,5,7-四氮杂环辛烷的合成研究

Synthesis study of 1,3,5,7-tetranitro-1,3,5,7-tetrazacyclo octane

以乌洛托品为原料,经过一步酰化合成中间体1,5-二乙酰基-3,7-桥亚甲基-1,3,5,7-四氮杂环辛烷(DAPT),再经过一步硝解合成中间体1,5-二乙酰基-3,7-二硝基-1,3,5,7-四氮杂环辛烷(DADN),并用红外光谱和元素分析进行表征。最后再用硝化剂硝化DADN的目标产物HMX合成1,3,5,7-四硝基-1,3,5,7-四氮杂环辛烷。结果表明:温度为0,反应时间为70 min合成DAPT;合成DADN的条件为温度18℃,反应时间1 h,硝酸铵与DADN的质量比3∶1,10 mL的发烟硝酸。实验以硝酸和氧化镁为组分的硝解组合,虽有较高的产率,但仍需继续研究以克服其纯度不高的问题。

With methenamine as raw materials,acylation synthesis of intermediate of 1,5-diacetyl-3,7-bridge methylene-1,3,5,7-tetraazacyclo octane（DAPT）and further nitration synthesis of intermediate of 1,5-diacetyl-3,7-dinitro-1,3,5,7-tetraazacyclo octane（DADN）were carried out,and the product was characterized by infrared spectroscopy and elemental analysis.Finally, nitration of the target product of HMX was performed with DADN nitrating agent. The results show that the synthesis conditions of DAPT：temperature 0,reaction time 70 min.Synthesis conditions of DADN：temperature 18 ℃,reaction time 1 h,the mass ratio ammonium nitrate and DADN 3∶1,the amount of fuming nitric acid 10 mL. Experiment with nitric acid and magnesium oxide as a component of the nitrolysis combinations,despite higher yield,but still need to continue to study in order to overcome the problem of high purity.