节点文献
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
【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