2,4-滴甲酯的合成工艺  

Synthesis of 2,4-D Methyl Ester

作　　者：付永丰 王达彤 徐婷 李培培[1] 岳涛 冯维春[1] FU Yong-feng;WANG Da-tong;XU Ting;LI Pei-pei;YUE Tao;FENG Wei-chun(Organic Reaction in Aqueous Engineering Research Center of Shandong Province,Qingdao University of Science&Technology,Jinan 250014,China)

机构地区：[1]青岛科技大学山东省水相有机合成及高效清洁分离工程技术研究中心,济南250014

出　　处：《农药》2020年第11期789-791,共3页Agrochemicals

基　　金：山东省政府“泰山学者”建设工程资金项目(08190201);山东省重大科技创新工程项目(2017CXGC1003)。

摘　　要：[目的]研究一种2,4-滴甲酯合成新工艺,解决现有工艺存在的溶剂使用量大、成本高、污染重、收率低等问题。[方法]以2,4-二氯酚和氯乙酸甲酯为主要原料,经过缩合反应合成2,4-滴甲酯,考察不同条件对2,4-滴甲酯收率的影响。[结果]表征结果表明,2,4-滴甲酯成功制备,产品收率高、质量好。[结论]通过二甲苯共沸带水,n(氯乙酸甲酯)∶n(2,4-二氯苯酚)为1.1∶1,缩合反应温度130℃,反应时间3 h,收率达97.6%(以2,4-滴甲酯计),纯度为99.2%(HPLC)。[Aims]This paper aims to study a new synthesis process of 2,4-D methyl ester to solve the problems of large solvent consumption,high cost,heavy pollution and low yield in the existing process.[Methods]Using2,4-dichlorophenol and methyl chloroacetate as the main raw materials,2,4-didymethyl ester was synthesized by condensation reaction,and the effect of different conditions on the yield of 2,4-didymethyl ester was investigated as well.[Results]The characterization results showed that 2,4-D methyl ester was successfully prepared with high yield and good quality.[Conclusions]The method of azeotrope of xylene and water was adopted to bring out water,the ratio of n(methyl chloroacetate)∶n(2,4-dichlorophenol)was 1.1∶1,the reaction was conducted at 130℃for 3 h,the yield was97.6%(calculated by 2,4-D methyl ester),and the purity was 99.2%(HPLC).

关 键 词：2 4-滴甲酯 2 4-二氯酚 氯乙酸甲酯 碱 

分 类 号：TQ460.3[化学工程—制药化工]