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3,6-二硝基吡唑[4,3-c]并吡唑的合成工艺改进

Improved Synthesis of 1H,4H-3,6-dinitropyrazolo[4,3-C] pyrazole

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【作者】 易文斌朱春琳王金星张怡蔡春

【Author】 YI Wen-bin,ZHU Chun-lin,WANG Jin-xing,ZHANG Yi,CAI Chun(Chemical Engineering College,Nanjing University of Science & Technology,Nanjing 210094,China)

【机构】 南京理工大学化工学院

【摘要】 3,6-二硝基吡唑[4,3-c]并吡唑(D N PP),是一种新型氮杂环含能材料。以乙酰丙酮为原料,经环化、重氮化、双环构建、硝化、氧化、脱羧硝化等反应合成了D N PP,得率为13.3%,比文献值提高了4%。考察了一锅法制备中间体4-氨基-3,5-二甲基吡唑的合成工艺、硝化工艺和脱羧硝化工艺。

【Abstract】 1H,4H-3,6-dinitropyrazolo[4,3-C] pyrazole(DNPP) was synthesized from acetylacetone via monocyclization,diazotization,bicyclization,nitration,oxidation,and decarboxylative nitration.The overall yield of DNPP was 11.3% and 4% higher than that reported before.The synthesis of 4-amino-3,5-dimethylpyrazole was carried out by one-pot method which shows a number of advantages in comparison with the procedure adapted in the literature,including eliminating the use of mixture acid and iron power,shorting the reaction time(from 72 h to 24 h),improving the yield(from 79.1% to 92.0%),and simplifying the post-treatment.In addition,both nitration and decarboxylative nitration were studied.

  • 【文献出处】 含能材料 ,Chinese Journal of Energetic Materials , 编辑部邮箱 ,2011年02期
  • 【分类号】TQ560.1
  • 【被引频次】5
  • 【下载频次】198
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