邓燕, 张永强, 何农跃, 蒋欢妹, 陶德良. 一锅法简便合成2,6-二甲基苯硼酸[J]. 信阳师范学院学报(自然科学版), 2011, 24(3): 394-396.
引用本文: 邓燕, 张永强, 何农跃, 蒋欢妹, 陶德良. 一锅法简便合成2,6-二甲基苯硼酸[J]. 信阳师范学院学报(自然科学版), 2011, 24(3): 394-396.
DENG Yan, ZHANG Yong-qiang, HE Nong-yue, JIANG Huan-mei, TAO De-liang. Preparation of 2,6-dimethylphenyl Boronic Acid by One-pot Grignard Reaction[J]. Journal of Xinyang Normal University (Natural Science Edition), 2011, 24(3): 394-396.
Citation: DENG Yan, ZHANG Yong-qiang, HE Nong-yue, JIANG Huan-mei, TAO De-liang. Preparation of 2,6-dimethylphenyl Boronic Acid by One-pot Grignard Reaction[J]. Journal of Xinyang Normal University (Natural Science Edition), 2011, 24(3): 394-396.

一锅法简便合成2,6-二甲基苯硼酸

Preparation of 2,6-dimethylphenyl Boronic Acid by One-pot Grignard Reaction

  • 摘要: 报道了2,6-二甲基苯硼酸的简便合成新方法.对硼化试剂、反应物比例、溶剂等条件进行了优化,优化后的合成条件为:选用硼酸三丁酯为硼化剂、四氢呋喃为溶剂,将加有2,6-二甲基溴苯、硼酸三丁酯物质量比(n(C8H9Br)∶n(B(OC4H9)3)为1∶1.5的四氢呋喃溶液滴加到1.2当量的镁屑中,于30℃一锅反应2 h后,经酸化水解得产品,分离后的总产率为80.1%.并对产品进行了1H NMR、质谱和IR表征.

     

    Abstract: A simple and convenient "one-pot" method is described for the preparation of 2,6-dimethylphenyl boronic acid.Parameters affecting preparation reaction including the boronation reagent,reactant proportion and solvent were investigated in detail.An optimized process was obtained when the solution of 2,6-dimethylphenyl bromide,tributyl borate and THF was added to the magnesium chip by drop,the reactant proportion was n(Mg)∶ n(C8H9Br)∶ n(B(OC4H9)3) = 1.2∶ 1∶ 1.5.The reactant solution was kept in a w...

     

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