SummaryI5N-CIDNP. spectra recorded during the reaction of diazonium cations with OH-in weakly alkaline aqueous solutions show that the dediazoniation is at least partially homolytic. The polarizations observed for the diazonium and transdiazotate ions can be explained by reaction proceeding via a cage involving diazenyl and diazotate radicals using Kuptein's rules and simple intensity considerations.