2-呋喃硼酸的合成研究

以2-溴呋喃和硼酸三丁酯为原料,采用正丁基锂法合成了2-呋喃硼酸。考察了反应温度、反应时间、物料配比以及pH值等主要因素对合成反应产率的影响。采用HPLC,FTIR,1 H NMR等方法对产品的纯度和结构进行了分析表征。结果表明:当反应温度为-60℃,反应时间为1h,物料配比为n(2-溴呋喃)∶n(硼酸三丁酯)∶n(正丁基锂)=1.00∶1.20∶1.20,pH值为6.0时,2-呋喃硼酸的产率最高可达84.0%,纯度可达99.702 7%。

Synthesis of 2-furanylboronic acid

2-furanylboronic acid was synthesized with 2-bromofuran and tributyl borate as raw materials by using the n-butyl lithium reagent method.The effects of reaction temperature,reaction time,reactant molar ratio and pH value on the reaction yield were investigated.The purity and structure of the product were characterized by HPLC,FTIR and 1H NMR.The optimal reaction condition for the synthesis of 2-furanylboronic acid was obtained as follows:the temperature is-60 ℃,the time is 1 h,the molar ratio is n(2-bromofuran)∶n(tributyl borate)∶n(n-butyl lithium)=1.00∶1.20∶1.20,and the pH is 6.0.Under the above reaction conditions,the yield of 2-furanylboronic acid reaches 84.0% and its purity is up to 99.702 7%.