高纯度2-溴苯并[9,10]菲的合成研究  

Synthesis of High Purified 2-Bromobenzo [9,10] phenanthrene

作　　者：段陆萌 陈婷 李仲庆 李继响 马则群 梁现丽 杭德余 DUAN Lu-meng;CHEN Ting;LI Zhong-qing;LI Ji-xiang;MA Ze-qun;LIANG Xian-li;HANG De-yu(Beijing Yanhua Jilian Optoelectronic Technology Co.,Ltd.,Beijing 102502,China;School of Chemistry and Chemical Engineering,Beijing Institute of Technology,Beijing 100081,China)

机构地区：[1]北京燕化集联光电技术有限公司,北京102502 [2]北京理工大学化学与化工学院,北京100081

出　　处：《化学试剂》2020年第11期1385-1389,共5页Chemical Reagents

摘　　要：标题化合物为有机发光、盘状液晶和生物医药等领域的重要中间体。高纯度的标题化合物的合成方法在文献中少有报道。以2-溴联苯为起始原料,先经过超低温锂化反应制成2-联苯硼酸,再与2,5-二溴硝基苯进行Suzuki偶联反应制得(2-硝基-4-溴苯基)-1,1′-联苯,所得产品再经过铁粉还原得到(2-氨基-4-溴苯基)-1,1′-联苯,最后使用亚硝酸异戊酯关环制得标题化合物。合成路线原料易得、操作简便、产品纯度高,适合工业化生产和市场高标准品质需求。化合物均经过氢谱和碳谱结构表征、高效液相色谱仪纯度测定,目标化合物还经过差示扫描量热法(DSC)和热重分析(TGA)测试性能。The target compound is an important intermediate in some fields such as organic luminescence,disk liquid crystal and biomedicine.The synthesis method of high purity target compound is rarely reported in literatures.2-biphenylboronic acid was prepared from the starting material 2-bromobiphenyl by lithiation reaction at ultra-low temperature,and then(2-nitro-4-bromophenyl)-1-1′-biphenyl was obtained from 2-biphenylboronic acid and 2,5-dibromonitrobenzene by Suzuki coupling reaction,which was reduced by iron powder to obtain(2-amino-4-bromophenyl)-1-1′-biphenyl,finally the title compound was prepared by ring closure with isoamyl nitrite.Synthetic route of the compound was easy to operate,and the raw materials were easy to obtain.The target compound was suitable for industrialization and market high standard quality demand because of high purity.The structures of the each step compound were confirmed by 1HNMR and 13CNMR,the purity was determined by HPLC,and the performance of target compound was tested by DSC and TGA.

关 键 词：2-溴苯并[9 10]菲 高纯度 有机电致发光材料 三亚苯 稠环化合物 

分 类 号：O626.13[理学—有机化学]