5-硝基-2H-四唑的合成、反应性及产物晶体结构的研究  

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

作　　者：孙成辉[1] 李玉川[1,2] 李亚裕[1,3] 李冠琼[2] 庞思平[1] 

机构地区：[1]北京理工大学材料学院,北京100081 [2]北京理工大学生命学院,北京100081 [3]北京航天试验技术研究所,北京100074

出　　处：《有机化学》2010年第3期424-430,共7页Chinese Journal of Organic Chemistry

基　　金：国家自然科学基金(No.20772011)资助项目

摘　　要：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-1.5-Nitro-2H-tetrazole （5） was prepared from 5-amino-lH-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 HC1 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, De=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 

分 类 号：O626.28[理学—有机化学]