2-氟-3-甲氧基-4-氯苯硼酸的合成新路线  

New synthesis route of(4-chloro-2-fluoro-3-methoxyphenyl)boronic acid

作　　者：刘长生 肖石基 蒋其柏 王鹏 LIU Chang-sheng;XIAO Shi-ji;JIANG Qi-bai;WANG Peng(Jiangsu BioGuide Laboratory Co.,Ltd.,Changzhou 213145,Jiangsu,China;BioGuide(Jiangsu)Laboratories Co.,Ltd.,Changzhou 213145,Jiangsu,China)

机构地区：[1]江苏乾元生物科技有限公司,江苏常州213145 [2]江苏百康德医药有限公司,江苏常州213145

出　　处：《农药》2023年第6期398-400,共3页Agrochemicals

摘　　要：[目的]探索2-氟-3-甲氧基-4-氯苯硼酸中间体的新合成路线。[方法]以副产品1-氯-2,3-二氟-5-硝基苯为起始原料,经由取代、氢化还原、溴代、重氮化脱氨基、格氏硼酸化制得中间体2-氟-3-甲氧基-4-氯苯硼酸。[结果]目标化合物的结构经^(1)H NMR确证,纯度为99%,收率为73.3%(以1-氯-2,3-二氟-5-硝基苯计)。[结论]确立了一种新的2-氟-3-甲氧基-4-氯苯硼酸中间体的合成方案,为大生产工艺提供了支撑。[Aims]The study aims to explore a new synthesis route of(4-chloro-2-fluoro-3-methoxyphenyl)boronic acid intermediate.[Methods]The intermediate of(4-chloro-2-fluoro-3-methoxyphenyl)boronic acid was synthesized from 1-chloro-2,3-difluoro-5-nitrobenzene via substitution reaction,hydrogenation reduction,bromination,diazotization and borination with Grignard reagent.[Results]The target compound was confirmed by^(1)H NMR,and the purity of it was 99%,while the total yield of it was 73.3%(based on 1-chloro-2,3-difluoro-5-nitrobenzene).[Conclusions]A new synthesis method of(4-chloro-2-fluoro-3-methoxyphenyl)boronic acid intermediate is established,which provides support for large-scale production process.

关 键 词：2-氟-3-甲氧基-4-氯苯硼酸 合成 氢化还原 硼酸化 条件优化 

分 类 号：TQ460.3[化学工程—制药化工]