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4,5-二氧代氰基咪唑盐酸盐的合成与表征

吴敏杰 李祥志 毕福强 李亚南 周彦水 王伯周

火炸药学报2017,Vol.40Issue(3):41-46,6.
火炸药学报2017,Vol.40Issue(3):41-46,6.DOI:10.14077/j.issn.1007-7812.2017.03.007

4,5-二氧代氰基咪唑盐酸盐的合成与表征

Synthesis and Characterization of 1H-imidazolium-4,5-dinitrile Dioxides Hydrochloride

吴敏杰 1李祥志 2毕福强 1李亚南 2周彦水 1王伯周2

作者信息

  • 1. 西安近代化学研究所,陕西 西安 710065
  • 2. 氟氮化工资源高效开发与利用重点实验室,陕西 西安 710065
  • 折叠

摘要

Abstract

Using 4,5-dicyanoiazole as starting material, a novel energetic compound 1H-imidazolium-4,5-dinitrile dioxides hydrochloride with total yield of 58.2% was self-designed and synthesized by addition reaction of hydroxylamine to cyanide, diazo-substitution reaction and hydrolysis reactions eliminating chlorine hydride.The structures of target compound and intermediates were characterized by IR, NMR and elemental analysis.Single crystal of the intermediate 4,5-dichloroximidoimidiazolium hydrochloride was cultured.The SHELXTL program was used to analyze the X-ray data of single crystal to get the structure parameters of crystal.Thermal decomposition property of 1H-imidazolium-4,5-dinitrile dioxides hydrochloride was studied by DSC.The results show that 4,5-dichloroximidoimidiazolium hydrochloride belongs to orthorhombic crystal system, the space group is Pna2(1), and molecular weight is 259.47 with density of 1.699 g/cm3.The exothermic reaction of 1H-imidazolium-4,5-dinitrile dioxides hydrochloride starts from 140.23℃ with two exothermic peaks at 162.73℃ and 177.73℃, and the exothermic reaction is ended at 208.48℃, showing that the structure of 1H-imidazolium-4,5-dinitrile dioxides hydrochloride is stable.

关键词

4,5-二氰基咪唑/4,5-二氧代氰基咪唑盐酸盐/氧化氰基化合物/热分解

Key words

4/5-dicyanoiazole/1H-imidazolium-4/5-dinitrile dioxides hydrochloride/nitrile oxide/thermal decomposition

分类

军事科技

引用本文复制引用

吴敏杰,李祥志,毕福强,李亚南,周彦水,王伯周..4,5-二氧代氰基咪唑盐酸盐的合成与表征[J].火炸药学报,2017,40(3):41-46,6.

基金项目

国家自然科学基金资助(No.21503162) (No.21503162)

火炸药学报

OA北大核心CSCDCSTPCD

1007-7812

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