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 k J/mol,热失重温度范围为209.17~398.67℃,累计热失重71.84%。
By using 4-nitroimidazole as a raw material in condensation with 2-amino-3,5-dinitro-6-chloropyridine and2,6-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 by1 H 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 k J /mol,while its mass loss of 71. 84% takes place at the temperature of 209. 17 ~ 398. 67 ℃.
出处
《爆破器材》
CAS
2016年第1期12-15,21,共5页
Explosive Materials
关键词
有机合成
含能化合物
热分解
4-硝基咪唑
organic synthesis
energetic compounds
thermal decomposition
4-nitroimidazole