二苯并–21–冠–7的合成与表征  

Synthesis and Characterization of Dibenzo-21-crown-7

作　　者：刘明明[1] 邓天龙[1] 高道林[1] 张楠[1] 余晓平[1] 

机构地区：[1]天津市海洋资源与化学重点实验室,天津科技大学海洋科学与工程学院

出　　处：《天津科技大学学报》2014年第6期36-40,共5页Journal of Tianjin University of Science & Technology

基　　金：国家自然科学基金资助项目(21276194)

摘　　要：采用经由中间体的两步法合成二苯并–21–冠–7,研究在氮气氛围下,反应时间、物料物质的量比和反应温度对合成双[2–(2–羟基苯氧基)乙基]醚中间体产率的影响;进一步研究在氮气氛围下,中间体与二氯三甘醇合成二苯并–21–冠–7的反应时间和反应温度对产率的影响.实验结果表明:回流时间为50,h、物料邻苯二酚和二氯乙基醚的物质的量比为2.5∶1、合成温度75,℃时,中间体的产率可达39.82%;在110,℃下中间体与二氯三甘醇回流反应25,h,二苯并–21–冠–7的产率为57.00%.采用显微熔点法确定合成产品的熔点范围,采用红外光谱、核磁共振氢谱(1H NMR)、质谱(MS)对合成的产品进行结构表征,结果表明本实验设计的合成方案切实可行.Dibenzo-21-crown-7（DB21C7）was synthesized with a two-step method via an intermediate. At the first step,the affecting factors including reaction time,temperature,the ratio of reactants for the yield of the intermediate double [2-（2-hydroxyl phenoxy）ethyl] ether under the nitrogen gas environment were investigated. And then,the influence of the back-flow time and temperature on the process of synthesizing DB21C7,using the intermediate and dichlorotriglycol in the nitro-gen gas environment was studied. The experimental results showed that the yield of the intermediate product was 39.82%under the optimal synthetic conditions：the molar ratio of catechol to dichloro-ethyl-ether was 2.5：1,the reaction time was 50,hours,and the temperature was 75,℃.The productivity of the target product DB21C7,was 57.00% under the optimal conditions of 25,hours of reacting time at 110,℃. In addition,the melting point range and physicochemical structure of DB21C7,was identified by using microscopic melting point meter,infrared spectrometer,1H,NMR and MS,and the results demonstrated that the synthetic method is feasible.

关 键 词：冠醚 邻苯二酚 中间体 二苯并-21-冠-7 合成 

分 类 号：O621.3[理学—有机化学]