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.
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)
出处
《化学试剂》
CAS
北大核心
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)。
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
diethyl malonate
alkylation reaction
2,2-bis(hydroxymethyl)butyric acid
reduction reaction
synthesis
