联苯-4-甲酸合成工艺研究

Research on the Synthesis of Biphenyl-4-Carboxylic Acid

以联苯和乙酰氯为原料,通过傅克酰基化反应合成4-联苯乙酮,在醋酸体系中,4-联苯乙酮经Co-Mn-Br常压催化氧化,得目标产物联苯-4-甲酸。详细考察了催化剂用量、物料配比、氧气流速和反应温度对氧化反应的影响,确定较佳的工艺条件:n(Co)∶n(Mn)=1∶1,n(Co+Mn)∶n(Br)=1∶1,催化剂的用量为1.5%(原料的重量比),氧气流速为150 m L/min,反应温度80℃。在此条件下,联苯-4-甲酸产品收率为92.9%(以原料联苯计),纯度为99.5%(HPLC面积归一化法)。产物结构经过熔点、1H-NMR和MS表征。

Biphenyl-4-carboxylic acid was synthesized from biphenyl and acetyl chloride by Friedel-crafts acyl reaction, Co-Mn-Br catalytic oxidation. The effects of reactions on the yield of biphenyl-4-carboxylic acid have been investigated and the optimized conditions are as follows： n（Co）∶n（Mn）=1∶1, n（Co＋Mn）∶n（Br）=1∶1, the usage of catalyst is 1.5 %（wt %）, the oxygen flow rate is 150 m L/min and the reaction temperature is 80 ℃. Under the optimized conditions, the yield of biphenyl-4-carboxylic acid can reach 92.9 % and the purity is higher than 99.5 %（HPLC area normalization method）. The obtained biphenyl-4-carboxylic acid has been identified by MP, 1H-NMR and MS.