The Sonogashira-Hagihara coupling of terminal acetylenes with aryl iodides in the presence of a nickel catalyst and CuI was investigated. The reaction proceeds rapidly in aqueous dioxane in the presence of Ni(PPh3)(2)Cl-2 with high yields of disubstituted tolanes being obtained. The reaction seems to be an inexpensive alternative to the palladium-catalyzed process. (C) 2003 Published by Elsevier Science Ltd.