Z. Yong, Xie Wei
2007
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Journal
Chinese Journal of Applied Chemistry
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.