[1]赵坤,刘祖亮.1-取代的4-硝基咪唑含能衍生物的合成、表征及热分解性能[J].爆破器材,2016,45(01):12-15，21.[doi:10.3969/j.issn.1001-8352.2016.01.003]
　ZHAO Kun,LIU Zuliang.Synthesis, Characterization and Decomposition of 1-Substitued 4-Nitroimidazole Energetic Derivatives[J].EXPLOSIVE MATERIALS,2016,45(01):12-15，21.[doi:10.3969/j.issn.1001-8352.2016.01.003]
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1-取代的4-硝基咪唑含能衍生物的合成、表征及热分解性能()
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《爆破器材》[ISSN:1001-8352/CN:32-1163/TJ]

卷:
45
期数:
2016年01
页码:
12-15，21
栏目:
基础理论
出版日期:
2016-01-29

文章信息/Info

Title:
Synthesis, Characterization and Decomposition of 1-Substitued 4-Nitroimidazole Energetic Derivatives
文章编号:
4929
作者:
赵坤; 刘祖亮
南京理工大学化工学院（江苏南京，210094）
Author(s):
ZHAO Kun;  LIU Zuliang
School of Chemical Engineering, Nanjing University of Science and Technology (Jiangsu Nanjing, 210094)
关键词:
有机合成; 含能化合物; 热分解; 4-硝基咪唑
Keywords:
organic synthesis;  energetic compounds;  thermal decomposition;  4-nitroimidazole
分类号:
TQ560.7
DOI:
10.3969/j.issn.1001-8352.2016.01.003
文献标志码:
A
摘要:
以4-硝基咪唑为原料，通过与2-氨基-3,5-二硝基-6-氯吡啶、2,6-二氯-3-硝基吡啶缩合，合成出未见文献报道的化合物6-(4-硝基-咪唑-1-基)-2-氨基-3,5-二硝基吡啶(1#)及6-氯-3-硝基-2-(4-硝基-咪唑-1-基)-吡啶(3#)，收率分别为65%、52%；并采用此种方法优化了3-硝基-2-(4-硝基-咪唑-1-基)-吡啶(2#)的合成，收率为85%。进一步尝试了化合物3#的叠氮化反应,得到5-叠氮基-6-硝基四唑基［1,5-a］吡啶(4#)。采用核磁共振、质谱、红外光谱、元素分析等方法对相关化合物的结构进行了表征。利用TG和 DSC分析法研究了化合物1#的热行为，结果表明：化合物1#的初始分解温度为221.83 ℃，分解放热总量为302.65 kJ/mol，热失重温度范围为209.17~398.67 ℃，累计热失重71.84%。
Abstract:
By using 4-nitroimidazole as a raw material in condensation with 2-amino-3,5-dinitro-6-chloropyridine and 2, 6-chloro-3-nitro-pyridine, 6-(4-nitro-imidazol-1-yl)-2-amino-3,5-dinitro-pyridine (1#) and 6-chloro-3-nitro-2-(4-nitro-imidazol-1-yl)-pyridine(3#) were synthesized with yields of 65% and 52% respectively. The synthesis of 3-nitro-2-(4-nitro-imidazol-1-yl)-pyridine (2#) was optimized by this method with a yield of 85%. Further azidation of compound 3# was carried on to give 5-azido-6-nitrotetrazolo ［1,5-a］pyridine(4#). The structures of these compounds were characterized by 1H NMR,13-C NMR, MS and elemental analysis. Thermal behavior of compound 1# was studied by TG and DSC. Results show that the initial decomposition temperature of compound 1# was 221.83℃, the total decomposition heat 302.65 kJ/mol, while its mass loss of 71.84% takes place at the temperature of 209.17~398.67 ℃.

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备注/Memo

备注/Memo:
收稿日期：2015-01-28
作者简介：赵坤（1988~），男，硕士，主要从事含能化合物合成及性能的研究。E-mail：zkmlgr@126.com
通信作者：刘祖亮（1951~ ），男，博导，研究员，主要从事含能材料制备、配方与应用技术研究。E-mail：njustlzl723@hotmail.com
更新日期/Last Update: 2016-01-28