5,6-二(2-甲氧基苯胺基)-2,3-吡啶二酮的合成和晶体结构

Synthesis and Crystal Structure of 5,6-Di(o-methoxylanilino)pyridine-2,3-dione

在无溶剂条件下,由3-羟基-2(1H)-吡啶酮与2-甲氧基苯胺在NaIO3作用下合成了5,6-二(2-甲氧基苯胺基)-2,3-吡啶二酮,其结构经1HNMR表征.采用X-射线单晶衍射仪测定了产物的晶体结构,晶体结构属单斜晶系,空间群P21/n,晶胞参数为:a=1.1655(2)nm,b=0.72080(10)nm,c=2.0326(4)nm,α=90°,β=92.17(3)°,γ=90°,V=1.7063(5)nm3,Z=4,F(000)=736,Mr=351.36,Dc=1.368g/cm3,μ=0.098mm-1,R1=0.0587,wR2=0.1365.

5,6-Di（o-methoxylanilino） pyridine-2,3-dione was synthesized via the reaction of 3-hydroxy-2 （ 1H ）- pyridinones with aromatic amine in the present of NaIO3 under solvent-free conditions by grinding. The structure of the product was characterized by ^1H NMR and X-ray single crystal diffraction： The crystal belongs to monoclinicsystem, it has the characters,space group P21/n with a = 1.165 5（2） nm, b = 0.720 80（10） nm, c = 2.032 6（4） nm, α= 90°, β= 92.17（3）°, γ= 90°, V =1.706 3 （5） nm^3, Z =4, F（000） =736, Mr = 351.36, Dc = 1.368 g/cm^3, μ= 0.098 mm^-1, R1=0.058 7, wR2 = 0.136 5.3figs.,2tabs., 10refs.