3-吡啶硼酸的合成研究  

Study of synthesis of 3-pyridyl boric acid

作　　者：刘国权[1] 梁九娣[1] 郭晓芝[2] 王海英[2] 韩建荣[1] 

机构地区：[1]河北科技大学理学院,河北石家庄050018 [2]石家庄市环境监测中心,河北石家庄050022

出　　处：《河北科技大学学报》2013年第5期426-429,共4页Journal of Hebei University of Science and Technology

基　　金：河北省自然科学基金(B2009000670)

摘　　要：以3-溴吡啶作为起始原料,与正丁基锂和硼酸三丁酯反应,制备了3-吡啶硼酸。考察了反应物配比、反应温度、反应时间、水解pH值对收率的影响。采用HPLC,FTIR,1 H NMR等方法对产品的纯度和结构进行了分析表征。实验结果表明:当反应温度为-65℃、反应时间为60min、物料配比为n(C5H4NBr)∶n(n-BuLi)∶n(B(OC4H9)3)=1.00∶1.20∶1.20、水解pH值为5.0时,3-吡啶硼酸的收率为82.20%,纯度可达99.50%以上。3-pyridylboronic acid is prepared by reactants of 3-bromopyridine C5H4NBr as a starting material,n-butyllithium（n-Buli）and tributylborate（B（OC4H9）3）.Effects of the mole ratio of reactants,reaction temperature,reaction time and pH on the yield were investigated.Purity and structure of the product were characterized by HPLC,FTIR and 1 H NMR.The optimal reaction conditions for the synthesis of 3-pyridylboronic acid are obtained as follows：-65 ℃,60 min,the molar ratio of 1.00∶1.20∶1.20（n（C5H4NBr）∶n（n-BuLi）∶n（B（OC4H9）3） and pH 5.0.Under the optimal conditions,the product yield and its purity can reach 82.20% and 99.50%,resgectively.

关 键 词：3-吡啶硼酸 正丁基锂 合成 

分 类 号：O626.11[理学—有机化学]