4,6-二硝基-5,7-二氨基苯并氧化呋咱(CL-14)的合成与表征  

Synthesis and Characterization of 4,6-Dinitro-5,7-diamino Benzenfuroxan(CL-14)

作　　者：王伯周[1] 霍欢[1] 李吉祯[1] 樊学忠[1] 刘愆[1] 

机构地区：[1]西安近代化学研究所,西安710065

出　　处：《有机化学》2011年第1期132-135,共4页Chinese Journal of Organic Chemistry

基　　金：国家973项目子专题(No.613740102)资助项目

摘　　要：以2,4,6-三硝基氯苯为原料,经过叠氮化、脱氮环化和异常亲核取代氢(VNS)反应合成了4,6-二硝基-5,7-二氨基苯并氧化呋咱(CL-14),三步总收率达到50.3%,并采用红外光谱、核磁共振光谱、元素分析等进行了结构表征;确定了合成CL-14的最佳VNS反应条件:以盐酸羟氨作为VNS试剂,20～40℃下反应6 h,收率达到60%(文献值53%).研究结果表明,CL-14具有良好的感度特性和热安定性,其撞击感度与中间产物4,6-二硝基苯并氧化呋咱(DNBF)基本相当,而其摩擦感度远低于其DNBF;DSC和TG-DTG实验发现,CL-14仅有一个分解过程,其分解峰温为308.52℃。4,6-Dinitro-5,7-diamino benzenfuroxan （CL-14） was synthesized from 2,4,6-trinitrchloroben- hzene through the process of azidcation, denitrogenation and vicarious nucleophilic substitution （VNS） reaction with total yield of 50.3%, and the structures of CL-14 and main intermediates were characterized by IR, NMR spectra and elemental analysis. The conditions of VNS reaction were optimized, and the optimal reactive conditions were obtained as follows： NH2OH·HCl was VNS reagent, the reactive time was 6 h at 20- 40 ℃, and the yield was reached to 60%. The experimental results showed that there were favorable mechanical sensitivities and thermal stability of CL-14, which friction sensitivity was better than that of DNBF. DSC and TG-DTG measurements indicated that there was only one decomposition process of CL-14 with exothermic peak temperature of 308.52 ℃.

关 键 词：合成 4 6-二硝基-5 7-二氨基苯并氧化呋咱(CL-14) 异常亲核取代氢(VNS)反应 性能 

分 类 号：O626.2[理学—有机化学]