引用本文:
张永强, 贺全国, 蒋欢妹, 邓燕, 谢维跃, 蒋佑清, 伍伟青. 2,6-二甲基苯硼酸制备方法的改进[J]. 应用化学,
2007, 24(10): 1216-1218.
Citation: ZHANG Yong-Qiang, HE Quan-Guo, JIANG Huan-Mei, DENG Yan, XIE Wei-Yue, JIANG You-Qing, WU Wei-Qing. An Improved Preparation Method of 2,6-Dimethylphenyl Boronic Acid[J]. Chinese Journal of Applied Chemistry, 2007, 24(10): 1216-1218.
Citation: ZHANG Yong-Qiang, HE Quan-Guo, JIANG Huan-Mei, DENG Yan, XIE Wei-Yue, JIANG You-Qing, WU Wei-Qing. An Improved Preparation Method of 2,6-Dimethylphenyl Boronic Acid[J]. Chinese Journal of Applied Chemistry, 2007, 24(10): 1216-1218.
2,6-二甲基苯硼酸制备方法的改进
English
An Improved Preparation Method of 2,6-Dimethylphenyl Boronic Acid
Abstract:
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.
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Key words:
- Grignard reagent
- / dimethylphenyl boronic acid
- / preparation
- / characterization
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