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

作　　者：易文斌[1] 朱春琳[1] 王金星[1] 张怡[1] 蔡春[1] 

机构地区：[1]南京理工大学化工学院,江苏南京210094

出　　处：《含能材料》2011年第2期156-159,共4页Chinese Journal of Energetic Materials

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。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.

关 键 词：有机化学 3 6-二硝基吡唑[4 3-c]并吡唑(DNPP) 1 4-二氨基-3 6-二硝基吡唑[4 3-c]并吡唑(LLM-119) 合成 

分 类 号：TQ560.1[化学工程—炸药化工]