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4-硝基吡唑的一锅两步法合成及其晶体结构
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(中北大学化工与环境学院, 山西 太原 030051)

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李永祥(1964-),男,教授,主要从事含能材料的合成与应用研究。e-mail: liyongxiang@nuc.edu.cn

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One-Pot Two Steps Synthesis of 4-Nitropyrazole and Its Crystal Structure
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(School of Chemical Engineering and Environment North University of China, Taiyuan 030051, China)

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    摘要:

    以吡唑为原料, 在98%发烟硝酸/20%发烟硫酸体系下通过一锅两步法合成了4-硝基吡唑(4-NP), 采用红外光谱、核磁共振波谱、高分辨质谱、元素分析等手段对目标产物进行了结构表征。用X-射线单晶衍射仪测定了其单晶结构。研究了物料比、反应温度、反应时间对产品收率的影响。结果表明, 较佳的合成工艺为: n(发烟硝酸) :n(发烟硫酸):n(浓硫酸):n(吡唑) =1.5:3:2.1:1, 反应温度为50 ℃, 反应时间1.5 h, 收率最高为85%。4-NP的单晶结构属于三斜晶系, 空间群为P-1, 晶胞参数为a=8.0329(11) Å, b=9.6305(8) Å, c=9.9036(8) Å, α=74.393(7)°, β=81.560(9)°, γ=83.196(9)°, V=727.40(13) Å3, Z=6, ρ=1.549 mg·mm-3, μ=0.132 mm-1, F(000)=348。

    Abstract:

    4-Nitropyrazole(4-NP) was synthesized via a "one-pot two steps" method using pyrazole as raw material in a fuming nitric acid (w=98%)/20% oleum system. The target product was characterized by IR spectrometry, nuclear magnetic resonance spectroscopy, high resolution mass spectrometry and elemental analysis. The single crystal structure was determined by X-ray single-crystal diffractometer The effect of material ratio, reaction temperature, and reaction time on the yield of product was studied. Results show that the best synthesis process is n(fuming nitric acid):n(oleum):n(concentrated sulfuric acid):n(pyrazole)=1.5:3:2.1:1, reaction temperature 50 ℃, reaction time 1.5 h, the highest yield is 85%. The single crystal structure of 4-NP belongs to triclinic crystal system, its space group is P-1 with cell paramaters of a=8.0329(11) Å, b=9.6305(8) Å, c=9.9036(8) Å, α=74.393(7)°, β=81.560(9)°, γ=83.196(9)°, V=727.40(13) Å3, Z=6, ρ=1.549 mg·mm-3, μ=0.132 mm-1, F(000)=348.

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李永祥,党鑫,曹端林,等.4-硝基吡唑的一锅两步法合成及其晶体结构[J].含能材料, 2018, 26(5):404-409. DOI:10.11943/j. issn.1006-9941.2018.05.005.
LI Yong-xiang, DANG Xin, CAO Duan-lin, et al. One-Pot Two Steps Synthesis of 4-Nitropyrazole and Its Crystal Structure[J]. Chinese Journal of Energetic Materials, 2018, 26(5):404-409. DOI:10.11943/j. issn.1006-9941.2018.05.005.

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历史
  • 收稿日期: 2017-09-22
  • 最后修改日期: 2017-11-17
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  • 在线发布日期: 2018-05-22
  • 出版日期: 2018-05-25