In the presence of a suitable nitroxide, 2-(t-butylazo)prop-2-yl hydroperoxide (la) decomposes cleanly into hydroxyl and t-butyl radicals; the rate constant for its disappearance in cyclohexane is given by: k = 9.58 x lO14exp.(-1.47 x lO4/T)sI. ... In order to pursue our investigations into the reactions of free radicals with polymerizable alkenes,' we required a clean, thermal source of hydroxyl radicals in organic solution. In this communication we describe the use of 2-( t- ...