3,4-二(4′-氨基-3′,5′-二硝基苯基)氧化呋咱的合成及热性能  

Synthesis and Thermal Performance of 3,4-Bis(4′-amino-3′,5′-dinitrobenzene-1′-yl)furoxan

作　　者：李亚南[1] 张志忠[1] 廉鹏[1] 王伯周[1] 杨威[1] 王友兵[1] 李辉[1] 

机构地区：[1]西安近代化学研究所,陕西西安710065

出　　处：《火炸药学报》2012年第3期18-22,共5页Chinese Journal of Explosives & Propellants

基　　金：国防基础产品创新计划科研(No.2371000415);国防科研基础计划项目(B09201100051)资助

摘　　要：以4-甲氧基苯腈为原料,经肟化、重氮化、脱氮、关环、硝化及胺化等六步反应合成3,4-二(4′-氨基-3′,5′-二硝基苯基)氧化呋咱(DANBF),并优化了肟化、氧化呋咱成环及硝化反应的条件,用DSC、TG等对目标化合物的热性能进行了表征。结果表明,氧化呋咱成环反应的最适宜条件为:Na2CO3摩尔量为理论摩尔量的1.35倍,反应温度2～10℃,反应时间5h,收率58.1%,纯度不小于99.0%(HPLC)。芳基取代的氧化呋咱化合物具有较好的热稳定性。3,4 Bis（4＇ amino-3＇, 5＇-dinitrobenzene-1 ＇-yl） furoxan was synthesized from 4-methoxybenzonitrile by six step reactions of oxime, diazotization, denitrification, cyclization, nitration and amination. The reaction conditions of oxime, eyclization and nitration were optimized and the thermal performance of the title compound was investigated by differential scanning calorimetry（DSC） and thermogravimetry（TG）. The results show that the optimum conditions of cyclization with yield of 58.1% and purity of 99.0%（HPLC） are that the amount of Na2CO3 is 1.35 times the calculation amount, reaction temperature 2-10℃, reaction time 5 h. The aryl substitutional furoxano compounds has good thermal stability.

关 键 词：有机化学 3 4-二(4’-氨基-3’ 5'-二硝基苯基)氧化呋咱 合成 热性能 

分 类 号：TJ55[兵器科学与技术—军事化学与烟火技术] TQ264[化学工程—有机化工]