2,6-二甲基苯硼酸制备方法的改进  

An Improved Preparation Method of 2,6-Dimethylphenyl Boronic Acid

作　　者：张永强[1] 贺全国[1] 蒋欢妹[1] 邓燕[1] 谢维跃 蒋佑清 伍伟青 

机构地区：[1]湖南工业大学绿色包装与生物纳米技术应用实验室,株洲412008 [2]湖南省轻工研究院

出　　处：《应用化学》2007年第10期1216-1218,共3页Chinese Journal of Applied Chemistry

基　　金：国家自然科学基金青年基金(20505020);湖南省教育厅科研基金(05C508);2005~2008湖南省普通高校青年骨干教师培养计划资助项目

摘　　要：选用硼酸三丁酯为硼化剂,利用格氏试剂法制备了2,6-二甲基苯硼酸,考察了温度、硼化试剂和反应物配比对产率的影响,得出了较佳的合成条件:先由0.1mol2,6-二甲基溴苯与0.12mol镁在43℃反应1.5h制得格氏试剂(产率98.2%),然后与0.2mol硼酸三丁酯在-10℃下发生亲核取代,2h快速升温至20℃,经酸性水解得产品,分离后总产率由有机锂法的51%提高到72.2%,且反应条件更加温和并对产品进行了核磁共振、质谱和IR表征。2,6-Dimethylphenyl boronic acid was prepared from tributyl borate and Grignard reagent. An optimized process was obtained by investigating the influence of temperature, boronization reagent and reactant proportion on the yield. Grignard reagent was prepared from 2,6-dimethylphenyl bromide and 0. 12 mol Mg at 43 ℃ in 1.5 h with a yield of 98. 2%, then it reacted with 0. 2 mol tributyl borate at - 10 ℃, and the reaction mixture was hydrolyzed in an acid medium after the temperature was increased to 20 ℃ in 2 h. The total yield is 72. 2%, which is much higher than that（51% ） of using organic lithium and the experimental conditions are more moderate. The product was characterized by ^1H NMR, mass spectrometry and IR.

关 键 词：格氏试剂 二甲基苯硼酸 制备 表征 

分 类 号：O627.3[理学—有机化学] O621.3[理学—化学]