Abstract Rigid polyaromatic dialdehydes: biphenyl??4, 4′??dialdehyde and its longer analogues have been synthesized in high yields by using the Suzuki–Miyaura cross?? coupling reaction. In addition, a novel procedure for a gram??scale preparation of biphenyl??4, 4′??dicarbaldehyde from commercially available 4, 4′??bis (chloromethyl) biphenyl has been developed.