A variety of 2,3-diiodinated biphenyl and iodinated meta-terphenyl derivatives were synthesized by a regioselective Suzuki-Miyaura cross-coupling reaction of 5-substituted 1,2,3triiodobenzenes. By using 1 equiv. of arylboronic acid, the Suzuki-Miyaura reaction yielded 2,3-diiodinated biphenyl derivatives with excellent regioselectivity. The coupling reaction predominantly occurred at the terminal position of the P. O.