2,2-二羟甲基丁酸的合成  

Synthesis of 2,2-Bis(hydroxymethyl)butyric Acid

作　　者：罗莎 蒋琳 金文斐 刀家普 袁明龙 LUO Sha;JIANG Lin;JIN Wen-fei;DAO Jia-pu;YUAN Ming-long(National and Local Joint Engineering Research Center for Green Preparation Technology of Biobased Materials,School of Chemistry&Environment,Yunnan Minzu University,Kunming 650500,China)

机构地区：[1]云南民族大学,化学与环境学院,生物基材料绿色制备技术国家地方联合工程研究中心,云南昆明650500

出　　处：《化学试剂》2020年第4期459-462,共4页Chemical Reagents

基　　金：国家自然科学基金青年基金资助项目(21302163)。

摘　　要：标题化合物是一种具有多官能团的新型功能性单体,可以广泛地应用于水性聚氨酯、聚酯、环氧树脂、涂饰剂工业等方面。为了优化其合成路线,以丙二酸二乙酯为原料,先在碱的催化下与溴乙烷发生烷基化反应;该单取代中间体再与甲醛进行羟甲基化反应,最后再经过单酯水解以及酯基还原共四步反应合成,总收率为66%。产物结构经1HNMR、13CNMR、MS确证。与已有的文献方法相比,报道的合成路线具有化学选择性好、操作简便、生产安全性好的特点。The title compound is a novel functional monomer with polyfunctional groups,which can be widely used in water polyurethane,polyester,epoxide resin,water-based finish,etc.In order to optimize the synthesis route,diethylmalonate is used as a raw material,and an alkylation reaction with bromoethane is carried out under the catalysis of sodium ethoxide.Then,the mono-substituted intermediate was hydroxymethylated with formaldehyde.Finally,hydrolysis followed by reduction was carried out to generate 2,2-bis(hydroxymethyl)butyric acid.Thus,the target product was synthesized in four successive steps with a total yield of 66%.The structure was confirmed by 1HNMR,13CNMR and MS.Compared with the reported synthetic routes,the protocol takes the advantage of high chemoselectivity,convenient operation and good safety.

关 键 词：丙二酸二乙酯 烷基化反应 2 2-二羟甲基丁酸 还原反应 合成 

分 类 号：O621.3[理学—有机化学]