5-三氟甲基-2-氯-4-吡啶硼酸的合成研究
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河北省自然科学基金(B2009000670)


Study on synthesis of 2-chloro-5-trifluoromethylpyridine-4-yl-boronic acid
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    摘要:

    采用2-氯-4-碘-5-三氟代甲基吡啶为起始原料,与正丁基锂溶液反应制备5-三氟甲基-2-氯-4-吡啶硼酸。实验研究了合成反应过程几种反应条件对合成产率的影响情况,采用HPLC,FTIR,1H 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-70 ℃,反应时间为2 h,反应物料配比n(2-氯-4-碘-5-三氟代甲基吡啶)∶n(硼酸三丁酯)∶n(正丁基锂)为1.00∶1.20∶1.20, 溶液pH值为9.0时,5-三氟甲基-2-氯-4-吡啶硼酸的收率为83.10%,纯度可达98.65%以上。

    Abstract:

    2-chloro-5-trifluoromethyl pyridine-4-yl-boronic acid was prepared with 2-chloro-4-iodo-5-trifluoromethyl pyridine as the raw material through reaction with n-butyl lithium reagent. Several reaction conditions of the synthesis process were studied through the experiment. The purity and structure of the products were characterized by HPLC, FTIR and 1H NMR. Experimental result shows that when the temperature is -70 ℃, the reaction time is 2 h, the molar ratio of n(C6H2ClF3IN)∶n(C12H27BO3)∶n(C4H9Li) is=1.00∶1.20∶1.20, and the pH is 9.0, the yield of 2-chloro-5-trifluoromethyl pyridine-4-yl-boronic acid reaches 83.10%, and its purity is up to 98.65%.

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刘国权,王闪闪,梁九娣,李秋武,韩建荣.5-三氟甲基-2-氯-4-吡啶硼酸的合成研究[J].河北科技大学学报,2014,35(4):330-333

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  • 收稿日期:2014-03-04
  • 最后修改日期:2014-04-23
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  • 在线发布日期: 2014-07-08
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