以联苯和草酰氯为原料,通过傅克酰基化反应合成联苯偶酰,在碱性条件下,叔丁基过氧化氢(TBHP)氧化联苯偶酰发生Bayer-villiger重排,得联苯二甲酸酐,经水解得目标产物联苯-4-甲酸。对酰化条件进行优化并详细考察了氧化试剂种类、物料配比、反应温度和时间对氧化收率的影响,并确定较佳的工艺条件:质量分数为70%叔丁基过氧化氢作为氧化试剂,联苯偶酰与氧化剂的物质的量比为1∶1.2,反应温度50℃,反应时间3h。在此条件下,联苯-4-甲酸产品收率为91.7%。产物经熔点、质谱、1 H NMR和13C NMR表征。 Biphenyl and oxalyl chloride were used as raw materials to synthesize biphenyl by Friedel-Crafts reaction. Under basic conditions, Bayer-villiger rearrangement of t-butyl hydroperoxide (TBHP) Phthalic anhydride, the hydrolysis of the target product biphenyl-4-carboxylic acid. The conditions of the acylation were optimized and the effects of the kind of the oxidant, the ratio of the materials, the reaction temperature and the time on the oxidation yield were investigated in detail. The optimum technological conditions were determined as follows: the mass fraction of 70% tert-butyl hydroperoxide Reagents, biphenyl and oxidant material ratio of 1: 1.2, the reaction temperature was 50 ℃, the reaction time 3h. Under these conditions, the yield of biphenyl-4-carboxylic acid was 91.7%. The product was characterized by melting point, mass spectrum, 1 H NMR and 13C NMR.