3,4-dinitropyrazole(DNP) was synthesized from pyrazole via N-nitration, rearrangement and C-nitration. N-nitration was improved for a safe synthesis of N-nitropyrazole and carried out by addition of pyrazole/acetic acid solution into nitric acid/acetic anhydride mixture. In addition, C-nitration conditions were optimized as follows:molar ratio of 3-nitropyrazole/nitric acid 1/2, nitration temperature 55-60 ℃, time 1 h. DNP′s total yield could be up to 55%, and purity 99%. The structures of the intermediate and the product were confirmed by IR, NMR, MS and element analysis.
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汪营磊,姬月萍,陈斌,等.3,4-二硝基吡唑合成与性能研究[J].含能材料,2011,19(4):377-379. WANG Ying-lei, JI Yue-ping, CHEN Bin, et al. Improved Synthesis of 3,4-Dinitropyrazole[J]. Chinese Journal of Energetic Materials,2011,19(4):377-379.