对氟苯硼酸的合成与表征

Synthesis and Characterization of p-Fluorophenylboronic Acid

采用格氏试剂法合成了对氟苯硼酸,通过红外、核磁等分析手段对产物进行了表征,并运用正交设计试验对影响其收率的诸因素进行分析,影响最大的为原料配比,其次是反应温度,得出优化合成条件为:对氟溴苯与硼酸三甲酯物质的量比为1:2,亲核取代温度为-20℃,反应时间为2h。在此条件下合成的目的产物的纯度为99.1%,总产物收率达60.1%。

the p-fluorophenylboronic acid was prepared by Grignard reagent technology. The above-prepared products were characterized by IR and IHNMR. The effects of reaction conditions on reaction yield were analyzed with the orthogonal experiment. It was found that the reactant molar ratio had the greatest effect, followed by the reaction temperature. The optimized conditions were obtained as follows： the reactant molar ratio of p-fluorobromobenzene to trimethyl borate was 1：2, the temperature for nucleophilic substitution was -20℃, and the reaction time was 2h. Under these conditions, the purity and yield of the product was 99.1% and 60.1 respectively.