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,Dc=1.754g/cm3,F(000)=128,μ=0.160mm-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 HCI or HBr to form 5-chlorotetrazole (7) and 5-bromotetrazole (8), re-spectively. Their structures were characterized by MS, IR, ~1H NMR and ~(13)C NMR techniques, and the crys-tal 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 P2_1, 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) nm~3, D_c= 1.754 g/cm~3, F(000)= 128,μ =0.160 mm~(-1).