2,6-二氨基-3,5-二硝基吡嗪-1-氧化物的合成及其晶体结构

Synthesis and Crystal Structure of 2,6-Diamino-3,5-dinitropyrazine-1-oxide

以三氟乙酸为溶剂和催化剂,2,6-二氨基-3,5-二硝基吡嗪与过氧化氢反应制备了2,6-二氨基-3,5-二硝基吡嗪-1-氧化物(LLM-105),其结构经1H NMR,IR,MS,元素分析和四圆单晶X-射线衍射仪表征。LLM-105属单斜晶系,空间群P21/n,晶胞参数:a=0.571 6(3)nm,b=1.593 5(5)nm,c=0.841 2(5)nm,α=90°,β=100.97(4)°,γ=90°,V=0.7522(6)nm3,Dc=1.908 g.cm-3,Z=4,μ=0.175 mm-1,F(000)=440,μ(MoKα)=1.047 mm-1;R1=0.053 2,wR2=0.137 9。LLM-105存在分子内和分子间氢键。

2,6-Diamino-3,5-dinitropyrazine-l-oxide（ LLM-105 ） was synthesized by reaction of 2,6- diamino-3,5-dinitropyrazine and hydrogen peroxide using trifluoroacetic acid as the solvent and catalyst. The structure of LLM-105 was characterized by ^1H NMR, IR, MS, elemental analysis and fourcircle single crystal X-ray diffraction. The crystal of LLM-105 belongs to monoclinic system, space group P 21/n with a =0.571 6（3） nm, b = 1.593 5（5） nm, c =0. 841 2（5） nm, α =90°,β = 100.97（4）°, γ=90°, V=0.7522（6） nm3 Dc=1.908 g·cm^-3, Z = 4, μ = 0.175 mm^-1 F（000） =440,/z（ Mo Ka） = 1. 047 mm^-1, R1 = 0.053 2, wR2 = 0. 137 9. There are intra- and inter-molecular hydrogen bonds in LLM-105 crystal.