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羧酸开环法合成1,1-二氨基-2,2-二硝基乙烯的研究
引用本文:蔡华强,舒远杰,黄辉,程碧波. 羧酸开环法合成1,1-二氨基-2,2-二硝基乙烯的研究[J]. 化学世界, 2005, 46(1): 41-46
作者姓名:蔡华强  舒远杰  黄辉  程碧波
作者单位:中国工程物理研究院化工材料研究所,四川,绵阳,621900;中国工程物理研究院化工材料研究所,四川,绵阳,621900;中国工程物理研究院化工材料研究所,四川,绵阳,621900;中国工程物理研究院化工材料研究所,四川,绵阳,621900
基金项目:中国工程物理研究院基金(20020540)资助课题
摘    要:对2一甲基咪唑为反应底物制备1,1一二氨基一2,2.二硝基乙烯(FOx一7)的合成方法进行了实验研究,找到了一种新的合成FOx.7的方法,该方法首次采用低碳有机羧酸与硝化中间体2一(二硝基亚甲基).4,5.咪唑烷二酮l的反应实现FOx一7的合成,对产物结构进行了表征并对反应奈件进行了优化。开环试剂为甲酸时,最优条件下两步反应(收率分别为20.3%和95.3%)的总收率约为19.3%,与氨水开环法(约13、1%)相比收率有较大幅度提高,通过控制反应时间和结晶时间可对FOx.7的颗粒度进行控制,同时该方法也是制备大颗粒和不同形貌特征FOx一7的有效方法。对开环反应机理进行了探讨,

关 键 词:2-(二硝基亚甲基)-4  5-咪唑烷二酮  1  1-二氨基-2  2-二硝基乙烯(FOX-7)  羧酸  合成  开环  反应机理
文章编号:0367-6358(2005)01-041-06

Study on Ring Cleavage of 2-(Dinitromethylene)-4,5-imidazolidinyldione to 1,1-Diamino-2,2-dinitroethylene by Carboxylic Acids
CAI Hua-qiang,SHU Yuan-jie,HUANG Hui,CHENG Bi-bo. Study on Ring Cleavage of 2-(Dinitromethylene)-4,5-imidazolidinyldione to 1,1-Diamino-2,2-dinitroethylene by Carboxylic Acids[J]. Chemical World, 2005, 46(1): 41-46
Authors:CAI Hua-qiang  SHU Yuan-jie  HUANG Hui  CHENG Bi-bo
Abstract:1,1-Diamino-2,2-dinitroethylene (FOX-7) was synthesized using 2-methylimidazole as raw material. Ring cleavage of 2-(dinitromethylene)-4,5-imidazolidine dione was achieved by reacting with carboxylic acids, and the reaction conditions were optimized. The overall yield of nitration and ring cleavage was 19.3%(about 13% in literature) when formic acid was used. The ring cleavage by carboxylic acids, methanol, water and aqueous ammonia was compared. The particle size of FOX-7 can be controlled by adjusting the reaction and crystallization time, and it is also an efficient method for the preparation of large particle size FOX-7 with different features. The reaction mechanism of ring cleavage was discussed.
Keywords:2-(dinitromethylene)-4  5-imidazolidinedione  carboxylic acids  synthesis  (1  1)-diamino-(2  2)-dinitroethylene(FOX-7)  ring cleavage  reaction mechanism
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