1,2-双(2'-甲氧基苯氧基)乙烷的制备与晶体结构

Synthesis and crystal structure of 1,2-bis( 2'-methoxyphenoxy) ethane

以邻羟基苯甲醚和1,2-二溴乙烷为原料,经取代反应合成了1,2-双(2'-甲氧基苯氧基)乙烷(1),并对其晶体结构进行了研究,它是合成开链聚醚类化合物的重要中间体。氢氧化钾与邻羟基苯甲醚反应形成酚钾盐,再与1,2-二溴乙烷发生取代反应,总收率92.2%。其结构经1H NMR、13C NMR、ESI-MS和IR表征。用单晶X射线衍射法测定了化合物1的晶体结构,晶体属单斜晶系,P21/n空间群,晶胞参数a=7.448(2),b=5.0320(16),c=18.693(6),β=92.575(8)°,V=699.9(4)3,Z=2,Dc=1.302 g/cm3,F(000)=292,μ=0.093 mm-1,R=0.0590,wR=0.1324(I>2σ(I)).

1,2-Bis(2′-methoxyphenoxy)ethane(1)was synthesized through substitution reaction,using 2-methoxyphenol and 1,2-dibromoethane as starting materials. The crystal structure was studied,which is an important intermediate in the synthesis of openchain polyether compounds. The potassium salt of 2-methoxyphenol phenol was obtained by potassium hydroxide and 2-methoxyphenol.The total yield was 92. 2%. The compound was characterized by 1 H NMR,13 C NMR,ESI-MS and IR. The crystal structure wasdetermined by X-ray single crystal diffraction method. The crystal belongs to monoclinic system with space group P21 / n,a =7. 448(2)?,b =5. 0320(16)?,c =18. 693(6)?,β =92. 575(8)°,V =699. 9(4)?3 ,Z =2,Dc =1. 302 g/ cm3 ,F(000)= 292,μ =0. 093mm-1 ,R =0. 0590,wR =0. 1324(I>2σ(I)).