A series of 4,4'-bis(alkyloxy/phenoxy methyl biphenyl)were synthesized,using 4,4'-bis(chloromethyl)-biphenyl(BCMB) as raw material by Williamson ether synthesis methods.The synthesis process of 4,4'-bis(methoxymethyl) biphenyl,4,4'-bis(butoxymethyl) biphenyl and 4,4'-bis(phenoxymethyl)biphenyl was improved in reaction time and yield.On the basis,a series of new compounds were prepared.