4-氯-3-羧基苯硼酸合成工艺的优化  

Process Optimization for the Synthesis of(4-chloro-3-carboxylphenyl) Boronic Acid

作　　者：滕明刚 柴慧芳[1] 赵春深[2] 段炼[1] 

机构地区：[1]贵阳中医学院药学院,贵州贵阳550002 [2]贵州大学药学院,贵州贵阳550025

出　　处：《广东化工》2015年第3期30-31,共2页Guangdong Chemical Industry

基　　金：贵州省社发攻关项目(黔科合SY字[2014]3054号);贵州省教育厅自然科学研究项目(黔教合KY字[2012]044号);贵州省高层次人才科研条件特助经费项目(TZJF-2010年-055号)

摘　　要：介绍了4-氯-3-羧基苯硼酸的合成工艺。以2-氯-5-溴甲苯为原料,与正丁基锂和硼酸三异丙酯反应、再经氧化得目标化合物。考察了反应物配比、反应时间和反应温度对收率的影响。采用HPLC,MS和1H NMR等方法对产品的纯度和结构进行了表征。实验结果表明:反应温度为-78℃,反应时间为1.5 h,物料比为n(C7H6Br F)∶n(n-u Li)∶n(B(Oi Pr)3)=1∶1.8∶1.2时,收率为96%。两步总收率为85%。本合成路线原料廉价易得、操作简单、后处理方便、生产周期短,适合工业化生产。To study the synthesis of（4-chloro-3-carboxylphenyl） boronic acid. Which was prepared from 4-bromo-1-chloro-2-methylbenzene through 2 steps like lithiation and oxidation to obtain the Target Product. Effects of the mole ratio of reactants, reaction temperature, reaction time and the yield were investigated.The structure of the Target Product was confirmed by MS, 1H-NMR and the optimal reaction conditions for the synthesis of（4- chloro-3-carboxylphenyl） boronic acid were obtained as follows,-78 ℃, 1.5 hours, the molar ratio of 1 ∶ 1.8 ∶1.2（n（C7H6Br F） ∶n（n- Bu Li） ∶n（B（Oi Pr）3））, under the optimal conditions the produc tyield and its purity can reach 96 %, and the total yield was 85 %. The synthetic process is applicable in industrial preparation with a lower cost and simplified operation.

关 键 词：2-氯-5-溴甲苯 4-氯-3-羧基苯硼酸 正丁基锂 合成 

分 类 号：TQ[化学工程]