1, 3-Dehydrobenzene, 1, 4-dehydrobenzene and 2, 3-dehydronaphthalene are generated in the thermal decomposition of appropriate diaryliodonium carboxylates as demonstrated by the use of the three phase test. Intermediate species C6H4CO2 for m-and p-benzyne and C10H6CO2 for 2, 3-naphthalyne have been unambiguously trapped in the same way, showing how non-concerted processes are the main pathway for generation of arynic ...