1-(4′-溴联苯-4-基)金刚烷的合成  

Synthesis of 1-(4'-Bromo-[1,1'-biphenyl]-4-yl)adamantine

作　　者：赵玮 邵晓红 孙建仁 潘文碧 温兴锋 陈潇 吕李章 温超群 高鋆 黄凯斌 廖飞飞 吴忠信 ZHAO We;SHAO Xiao-hong;UN Jan-ren;PAN Wen-bi;WEN Xing-feng;CHEN Xio;LU Li-zhang;WEN Chao-qun;GAO Jun;HUANG Kai-bin;LIAO Fei-fei;WU Zhong-xin(Wenzhou Institute of Industry&Science,Wenzhou 325028,China;Zhejiang Huaji Biotechnology Co.,Ltd.,Wenzhou 325024,China;Zhejiang Engineering Research Center of New Organic Functional Molecules Synthesis and Application,Wenzhou 325028,China)

机构地区：[1]温州市工业科学研究院,浙江温州325028 [2]浙江华基生物技术有限公司,浙江温州325024 [3]浙江省新型有机功能分子合成与应用工程技术中心,浙江温州325028

出　　处：《精细化工中间体》2023年第6期48-51,共4页Fine Chemical Intermediates

基　　金：温州市重大科技创新攻关项目(揭榜挂帅)(ZG2023038)。

摘　　要：以1-溴金刚烷与4-溴联苯为原料,经Friedel-crafts烷基化反应制备了1-(4′-溴联苯-4-基)金刚烷。优化工艺为:反应温度25℃,反应时间24 h,1,2-二氯乙烷为溶剂,浓硫酸为催化剂,n(1-溴金刚烷)∶n(4-溴联苯)∶n(浓硫酸)=1.0∶1.0∶1.5。优化条件下目标化合物收率84.3%,纯度99.5%。目标化合物的结构经碳谱以及气相质谱表征确证。该制备方法原料易得,反应路线简单,反应条件温和,收率高,纯化处理简便,为1-(4′-溴联苯-4-基)金刚烷的工业化生产提供了新的途径。1-(4'-Bromo-[1,1'-biphenyl]-4-yl)adamantane was prepared by Friedel-Crafts alkylation reaction using 1-bromoadamantane and 4-bromobiphenyl as raw materials.The process was optimised as followings:reaction temperature 25 C,reaction time 24 h,1,2-dichloroethane solvent,sulphuric acid as catalyst,n(1-bromoadamantane):n(4-bromobiphenyl):n(sulphuric acid)=1.0:1.0:1.5.The yield of the target compound under the optimised conditions was 84.3%with a purity of 99.5%.The structure of the compound was characterized by'H NMR,13C NMR and GC-MS.This preparation method had the advantages of easy availability of raw materials,simple reaction route,mild reaction conditions,high yield and easy purification.It provided a new approach for the industrial production of 1-(4'-bromo-[1,1'-biphenyl]-4-yl)adamantane.

关 键 词：1-(4′-溴联苯-4-基)金刚烷 FRIEDEL-CRAFTS烷基化反应 合成 

分 类 号：TQ241.3[化学工程—有机化工]