2,4,7,9-四硝基-2,4,7,9-四氮杂双环[4,3,0]壬酮合成工艺改进

Technical Improvement for Synthesizing 2,4,7,9- tetranitro-2,4,7,9-tetrazabicyclo [4,3,0] nonanone

以乙二胺、乙二醛和脲为原料 ,合成了 2 ,4 ,7,9-四氮杂双环 [4,3,0 ]壬酮盐酸盐 ( 1 ) ,通过改变加料顺序 ,反应得率提高到 76 .1 %。化合物 ( 1 )在硝酸 -乙酐体系中硝化 ,制得 2 ,4 ,7,9-四硝基 - 2 ,4 ,7,9-四氮杂双环 [4,3,0 ]壬酮 ( 2 ) ,通过优化反应工艺条件 ,反应得率增加到 6 5.9%。合成化合物 ( 2 )的总得率为50 .1 % ,熔点 1 94～ 1 96℃。文中初步了分析了合成化合物 ( 1 )的缩合反应的机理和主要影响因素 ,讨论了化合物 ( 1 )

The technical improvement for the synthesis of 2,4,7,9-tetrazabicyclononanone hydrochlorate(1) from ethylenediamine, glyoxal and urea was reported.The yield of compound (1) increased to 76.1 % with the order chang of adding matter. By nitration of the compound (1) with nitric acid in acetic anhydride, 2,4,7,9-tetranitro-2,4,7,9-tetrazabicyclononanone (2) was given, the yield of compound (2) increased to 65.9 % with the optimization of technical condition. The total yield of compound (2) is 50.1 %.The melting point of compound (2) is 194～196 ℃. The mechanism of condensation reaction for synthesizing compound (1) and the main factors affecting the yield of condensation reaction were analyzed. As for the nitration reaction of compound (1), the factors and the mechanism of nitration reaction are also discussed.