节点文献
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
【摘要】 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)).
【Abstract】 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 open chain 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 by1 H NMR,13 C NMR,ESI-MS and IR. The crystal structure was determined 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)).
【Key words】 open-chain polyether; 1,2-Bis(2’-methoxyphenoxy) ethane; synthesis; crystal structure;
- 【文献出处】 化学研究与应用 ,Chemical Research and Application , 编辑部邮箱 ,2016年08期
- 【分类号】O621.3
- 【被引频次】1
- 【下载频次】61