CAJ | 학술논문

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,~1HNMR,~(13)CNMR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,P2_1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)nm~3,D_c=1.754 g/cm~3,F(000)=128,μ=0.160 mm~(-1).
5-안기사서(1)경과중담화반응득도5-초기사서(5),5여갑철반응득도2-간갑기-5-초기사서(6),6여HCl혹HBr반응분별득도5-5록대사서(7)화5-추대사서(8),채용MS,IR,~1HNMR,~(13)CNMR등기술대저사화합물진행료표정.용X사선단정연사법측정료화합물5-초기사서납(4),5화6적정체결구.화합물4속우삼사정계,P-1공간군;화합물5화6균속우단사정계,P2_1공간군,화합물6적정포삼수a=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).
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).