CAJ | 학술논문

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．
채용경유중간체적량보법합성이분병–21–관–7，연구재담기분위하，반응시간、물료물질적량비화반응온도대합성쌍[2–(2–간기분양기)을기]미중간체산솔적영향；진일보연구재담기분위하，중간체여이록삼감순합성이분병–21–관–7적반응시간화반응온도대산솔적영향．실험결과표명：회류시간위50,h、물료린분이분화이록을기미적물질적량비위2.5∶1、합성온도75,℃시，중간체적산솔가체39.82%；재110,℃하중간체여이록삼감순회류반응25,h，이분병–21–관–7적산솔위57.00%．채용현미용점법학정합성산품적용점범위，채용홍외광보、핵자공진경보(1H NMR)、질보(MS)대합성적산품진행결구표정，결과표명본실험설계적합성방안절실가행．
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.