| 3-吡啶硼酸的合成研究 |
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| 引用本文： | 刘国权,梁九娣,郭晓芝,王海英,韩建荣.3-吡啶硼酸的合成研究[J].河北科技大学学报,2013,34(5):426-429. |
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| 作者姓名： | 刘国权 梁九娣 郭晓芝 王海英 韩建荣 |
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| 作者单位： | [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 |
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| 基金项目： | 河北省自然科学基金（B2009000670） |
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| 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。
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| 关 键 词： | 3-吡啶硼酸 正丁基锂 合成 |
Study of synthesis of 3-pyridyl boric acid |
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| LIU Guoquan,LIANG Jiudi,GUO Xiaozhi,WANG Haiying and HAN Jianrong.Study of synthesis of 3-pyridyl boric acid[J].Journal of Hebei University of Science and Technology,2013,34(5):426-429. |
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| Authors: | LIU Guoquan LIANG Jiudi GUO Xiaozhi WANG Haiying and HAN Jianrong |
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| Institution: | 1. School of Science, Hebei University of Science and Technology, Shijiazhuang Hebei 050018, China; 2. Shijiazhuang Environmental Monitoring Centre, Shijiazhuang Hebei 050022, China) |
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| Abstract: | 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. |
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| Keywords: | 3-pyridylboric acid n-butyllithium synthesis |
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