芴基硼酸酯的连续流合成工艺研究  

Study on continuous flow synthesis process of fluorenyl boronate

作　　者：魏颖 李晓艳 包秋景 高月正 陶房菊 WEI Ying;LI Xiaoyan;BAO Qiujing;GAO Yuezheng;TAO Fangju(Faculty of Materials Science and Engineering,Nanjing University of Posts and Telecommunications,Nanjing 210023,China)

机构地区：[1]南京邮电大学材料科学与工程学院,江苏南京210023

出　　处：《实验室科学》2024年第4期37-41,共5页Laboratory Science

基　　金：国家自然科学基金(项目编号:2207112);江苏省高校自然科学研究面上项目(项目编号:20KJB150038)。

摘　　要：将科研成果“芴基硼酸酯的连续流合成工艺研究”转化为材料专业的本科综合性实验。实验根据间歇法合成硼酸酯的条件设计了连续流硼化反应的路线,通过控制变量法对停留时间、温度、溶剂等进行了条件优化,确定了连续流合成芴基硼酸酯的最佳工艺条件:溶剂为二甲亚砜、停留时间为58 s,浓度0.2 M、温度为150℃、n(2-溴-9-苯基芴醇)∶n(联硼酸频那醇酯)∶n(碱液)=1∶1.5∶3,产物9-苯基芴醇硼酸酯(FOHBin)的产率为87.4%。The scientific research achievement“Study on the Continuous Flow Synthesis of Fluorenyl Boronate”was transformed into a comprehensive undergraduate experiment in materials major.The experiment designed a continuous flow boronation reaction route according to the conditions of the batch method for synthesizing boronic esters,and optimized the conditions of residence time,temperature and solvent by controlling the variable method,and determined the optimal continuous flow synthesis of fluorenyl boronic esters.Process conditions:the solvent is dimethyl sulfoxide,the residence time is 58s,the concentration is 0.2M,the temperature is 150℃,n(2-bromo-9-phenyl-9H-fluoren-9-ol):n(bis(pinacolato)diboron):n(alkali liquor)=1:1.5∶3,the yield of the product 9-phenyl-2-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-9 H-fluoren-9-ol(FOHBin)was 87.4%.

关 键 词：连续流技术 微通道反应器 芴 硼化反应 

分 类 号：G482[文化科学—教育学]