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有机化学
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有机化学 ›› 2010, Vol. 30 ›› Issue (03): 424-430. 上一篇    下一篇

研究论文

5-硝基-2H-四唑的合成、反应性及产物晶体结构的研究

孙成辉a，李玉川a,b，李亚裕a,c，李冠琼b，庞思平*,a   

  1. (a北京理工大学材料学院 北京 100081)
    (b北京理工大学生命学院 北京 100081)
    (c北京航天试验技术研究所 北京 100074)
  • 收稿日期:2009-09-27 修回日期:2009-11-22 发布日期:2010-03-28
  • 通讯作者: 李玉川 E-mail:yuchuanyh@yahoo.com.cn
  • 基金资助:

    国家级.国家自然科学基金

Study on Synthesis and Reactivity of 5-Nitro-2H-tetrazole and Crystal Structrue of Some Products

Sun Chenghuia,Li Yuchuana,b,Li Yayua,c,Li Guanqiongb,Pang Siping*,a   

  1. (a School of Material Science and Engineering, Beijing Institute of Technology, Beijing 100081)
    (b School of Life Science and Technology, Beijing Institute of Technology, Beijing 100081)
    (c Beijing Institute of Aerospace Testing Technology, Beijing 100081)
  • Received:2009-09-27 Revised:2009-11-22 Published:2010-03-28
  • Contact: LI Yu-Chuan E-mail:yuchuanyh@yahoo.com.cn

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5-氨基四唑(1)经过重氮化反应得到5-硝基四唑(5), 5与甲醛反应得到2-羟甲基-5-硝基四唑(6), 6与HCl或HBr反应分别得到5-5氯代四唑(7)和5-溴代四唑(8), 采用MS, IR, 1H NMR, 13C NMR等技术对这些化合物进行了表征. 用X射线单晶衍射法测定了化合物5-硝基四唑钠(4), 5和6的晶体结构. 化合物4属于三斜晶系, P-1空间群; 化合物 5和6均属于单斜晶系, P21空间群, 化合物6的晶胞参数a＝0.66131(18) nm, b＝0.54905(15) nm, c＝0.7566(2) nm, Z＝2, V＝0.27470(13) nm3, Dc＝1.754 g/cm3, F(000)＝128, μ＝0.160 mm－1.

关键词: 硝基四唑, 合成, 晶体结构, 反应性

5-Nitro-2H-tetrazole (5) was prepared from 5-amino-1H-tetrazole (1) through diazotization and Sandmeyer reaction. 5 was then reacted with formaldehyde to form 5-nitro-2-hydroxymethyl-tetrazole (6), and 6 was reacted with concentrated HCl or HBr to form 5-chlorotetrazole (7) and 5-bromotetrazole (8), respectively. Their structures were characterized by MS, IR, 1H NMR and 13C NMR techniques, and the crystal structures of 5-nitrotetrazole sodium salt (4), 5 and 6 were determined by X-ray single crystal diffraction analysis. 4 belongs to triclinic system with space group P-1; 5 and 6 belong to monoclinic system with space group P21, and the crystal parameters of 6 were a＝0.66131(18) nm, b＝0.54905(15) nm, c＝0.7566(2) nm, Z＝2, V＝0.27470(13) nm3, Dc＝1.754 g/cm3, F(000)＝128, μ＝0.160 mm－1.

Key words: nitrotetrazole, synthesis, crystal structure, reactivity