摘要
以5-溴-1,2,3-三氟苯为原料,经氰化取代,甲氧基化,氰基酸性水解,霍夫曼降级重排,重氮化和Gattermann反应,高效合成了5-溴-1,3-二氟-2-甲氧基苯,其结构经1H NMR,13C NMR和MS(EI)确证。并利用气相色谱(GC)和高效液相色谱(HPLC)实时监测反应进程,优化了合成条件。
5-Bromo-1,3-difluoro-2-methoxybenzene was efficiently synthesized by cyanation,methoxylation,acid-promoted hydrolyzation,Hofmann rearrangement,aniline diazotization and Gattermann reaction,using 5-bromo-1,2,3-trifluorobenzene as the starting material. The structure was confirmed by1 H NMR,13 C NMR and MS( EI). In addition,the reaction progress was monitored by GC and HPLC to optimize the reaction conditions.
作者
黄琳
彭宏英
刘钢
程华
陈宬
HUANG Lin;PENG Hong-ying;LIU Gang;CHENG Hua;CHEN Cheng(Department of Chemical Engineering and Food Science,Hubei University of Xiangyang 441053,China;State Key Laboratory of Advanced Technology for Materials Synthesis and Processing,Wuhan University of Technology,Wuhan 430070,China)
出处
《合成化学》
CAS
CSCD
北大核心
2018年第6期433-436,共4页
Chinese Journal of Synthetic Chemistry
基金
国家自然科学基金青年基金资助项目(21502062)
中央高校基本科研业务费专项资金资助项目(2017IVA091)
湖北省教育厅项目(Q20102606)
襄阳市科技局项目(2010GG1B33)
食品新型学科群开放课题