3-[(2,3-二氢噻吩并[3,4-b]-1,4-二噁英-2-基)甲氧基]-丙酸的合成工艺改进  

Improved Synthesis of 3-[(2,3-Dihydrothieno[3,4-b][1,4]dioxin-2-yl)methoxy]propanoic Acid

作　　者：马晓莉 刘春晖 江志波 郭鑫 MA Xiao-li;LIU Chun-hui;JIANG Zhi-bo;GUO Xin(School of Chemistry and Chemical Engineering,North Minzu University,Yinchuan 750021,China)

机构地区：[1]北方民族大学化学与化学工程学院,宁夏银川750021

出　　处：《化学试剂》2021年第2期256-258,共3页Chemical Reagents

基　　金：宁夏自然科学基金项目(2019AAC03113);宁夏高等学校科学研究项目(NGY2017165);北方民族大学重大专项项目(ZDZX201803)。

摘　　要：报道了一种合成标题化合物的新工艺。以噻吩并[3,4-b]-1,4-二噁英-2-甲醇为起始原料,与丙烯酸叔丁酯发生迈克尔加成反应得到中间体化合物3-[(2,3-二氢噻吩并[3,4-b]-1,4-二噁英-2-基)甲氧基]丙酸叔丁酯。将得到的中间体在碱性条件下进行水解反应,然后采用盐酸进行酸化,最终经过干燥、减压浓缩、洗脱等后处理得到合格的标题化合物,总产率为71.2%,标题化合物及中间体经^(1)HNMR确认结构。路线操作简便、反应条件温和、产品质量可控,具有一定的工业应用意义。A new process for the synthesis of title compound was reported.Using[3,4-b]-1,4-dioxin-2-methanol as the starting material,it was reacted with tert-butyl acrylate to give 3-[(2,3-dihydrothiophene[3,4-b]-1,4-dioxin-2-yl)methoxy]propionic acid tert-butyl ester.The ester was hydrolyzed under alkaline conditions,then was acidified with hydrochloric acid.The final sample was undergo post-treatments such as drying,vacuum distillation and elution to obtain a high purity title compound,the yield was 71.2%.The title compound and intermediate compound were confirmed by ^(1)HNMR.The route has the advantages of simplified operation,mild reaction conditions and controllable product quality,and has certain industrial value.

关 键 词：3-[(2 3-二氢噻吩并[3 4-b]-1 4-二噁英-2-基)甲氧基]-丙酸 丙烯酸叔丁酯 合成 工艺 改进 迈克尔加成反应 

分 类 号：TQ463[化学工程—制药化工]