The o-iodobiphenylyl ethers 4, 5, 9, and 18 from cyclododecanol, 1-dodecanol, l,2:3,4-di-0-isopropylidene--D-galactopyranose, and l,2:5,6-di-0-isopropylidene-a-D-glucofuranose, respectively, were synthesized by tosylate (compounds 4, 5, and 9) or triflate (compounds 9 and 18) displacement by the anion of 2-iodo-4-phenylphenol. Alkene formation, which always was accompanied by formation of the unsubstituted biphenylyl ether (iodine replaced by hydrogen), resulted from photolysis of compounds 4, 5, and 9 in 2-methyl-2-propanol. Irradiation of 18 produced only the unsubstituted biphenylyl ether 19.