镁离子催化下2-(二硝基亚甲基)-1,3-二氮环戊烷的合成

Synthesis of 2-(Dinitromethylene)-1,3-diazacyclopentane(DNDZ) Catalyzed by Magnesium Ion

2-(二硝基亚甲基)-1,3-二氮戊烷(DNDZ)是设计合成新型含能材料关键的中间体,本研究考察了镁离子催化下1,1-二氨基-2,2-二硝基乙烯(FOX-7)与乙二胺进行的亲核反应,确定了合成DNDZ的最佳反应条件:反应温度为110℃、反应时间为5.5h,Mg(OAc)2作为催化剂且用量为FOX-7物质的量的30%,DNDZ的产率为83.9%,纯度为99%。并采用红外光谱、核磁共振波谱、质谱以及元素分析等进行了结构表征。

As an important intermediate for new energetic materials, 2-（dinitromethylene）-1, 3-diaza-cyclopentane（DNDZ） attracts more attentions in recent years. Herein the necleophilic reaction between 1 ,1-diamino-2,2-dinitroethylene（FOX-7） and 1 ,2-diaminoethane catalyzed by magnesium ion was studied and the DNDZ was synthesized in yield of 83,9% with high purity （99%） under the optimum conditions, the reaction temperature and time were 110 ℃ and 5.5 h respectively and the best catalyst was new prepared Mg（OAc）2（30%）. The structure of the product was characterized by IR, NMR, MS and elemental analysis.