B-[9,9-双(4-甲基苯基)-9H-芴-2-基]硼酸的合成工艺优化  

Process Improvement on Synthesis of B-[9,9-bis(4-methyl-phenyl)-9H-fluoren-2-yl]boric Acid

作　　者：邓浩 刘彤[1] 廖万鹏 吴凤 DENG Hao;LIU Tong;LIAO Wan-peng;WU Feng(College of Chemistry and Chemical Engineering, Guizhou University, Guiyang 550025, China)

机构地区：[1]贵州大学化学与化工学院,贵州贵阳550025

出　　处：《合成化学》2021年第4期327-331,共5页Chinese Journal of Synthetic Chemistry

基　　金：贵州省科技合作计划项目(黔科合LH字[2017]7252号);贵州省科技计划社发发展科技攻关项目(黔科合SY字[2013]3092号,SY字[2013]3079号,SY字[2014]3052号);贵州大学2017年度学术新苗培养及创新探索专项(黔科合平台人才[2017]5788号)。

摘　　要：以2-溴-9-芴酮为原料,经亲核加成、取代、氧化还原、氧化反应合成B-[9,9-双(4-甲基苯基)-9H-芴-2-基]硼酸,其结构经^(1)H NMR确证。采用响应面法重点对氧化还原步骤进行优化。确定较优合成条件为:反应时间5.4 h,催化剂用量为0.4 eq.,反应温度为108℃,目标产物收率92.15%,相对误差0.54%。Using 2-bromo-9-fluorenone as raw material,B-[9,9-bis(4-methylphenyl)-9H-fluorene-2-yl is prepared through nucleophilic addition,substitution,redox and oxidation reactions.The response surface method was used to optimize the redox steps.The optimum process conditions were determined as followed:the catalyst dosage was 0.4 eq,reaction was carried out at 108℃for 5.4 h,and target product yield was 92.15%,relative error 0.54%,indicating that the model was reliable and effective.The significance test results of the regression model indicated that the order of the degree of influence on the response value was catalyst dosage>reaction temperature>reaction time.

关 键 词：B-[9 9-双(4-甲基苯基)-9H-芴-2-基]硼酸 合成 工艺优化 响应面法 加成 取代 

分 类 号：TQ242.9[化学工程—有机化工] O62[理学—有机化学]