5-硝基-2H-四唑的合成、反应性及产物晶体结构的研究

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, D_c＝1.754 g/cm³, F(000)＝128, μ＝0.160 mm^－1.

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

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, D_c＝1.754 g/cm³, F(000)＝128, μ＝0.160 mm^－1.