联苯双酯合成中Ullmann反应催化剂的研究  

Research on the Catalyst for Ullmann Reaction in Synthesis of Biphenyldicarboxylate

作　　者：梁永瑞 宋丽雪 

机构地区：[1]沈阳石油化工设计院,辽宁沈阳110044 [2]辽宁省医药规划设计院有限公司,辽宁沈阳110001

出　　处：《辽宁化工》2012年第5期442-443,446,共3页Liaoning Chemical Industry

摘　　要：对联苯双酯的合成工艺进行了研究,针对最后一步Ullmann反应催化剂铜粉的活化进行了大量的探索,希望能提高铜粉的活性,缩短Ullmann反应时间,进一步减低成本。以没食子酸为原料,经酯化、单甲醚化、邻双羟基的次甲二氧基化、溴化和Ullmann反应,共五步反应制得联苯双酯,总收率为30.2%,TLC显示纯度较好,并经TLC和IR确证结构正确。The synthesis process of biphenyldicarboxylate was studied.In order to improve activity of the copper powder and shorten Ullmann reaction time to decrease cost,activity of copper powder catalyst for Ullmann reaction was discussed.Biphenyldicarboxylate was synthesized from gallic acid via five steps including esterifying,single etherifying of methyl ether,forming of methenyldioxo group,bromation and Ullmann reation.It was corroborated structurally by IR and 1HNMR.Total yield is 30.2%.Its purity is good at TLC.

关 键 词：联苯双酯 铜粉活化 ULLMANN反应 合成 保肝药 

分 类 号：TQ426[化学工程]