The synthesis of various new trialkylhydroxylamines is described. The rate constant of the CO bond cleavage of these new alkoxyamines has been measured. For example, CO bond homolysis rates in a series of para-substituted TEMPO-styryl compounds TEMPO-CH (CH3) C6H5X 1a (p-MeO), 1b (p-Me), 1d (pH), 1e (p-Br), and 1f (p-MeO2C) are presented. Furthermore, rate constants for the CO bond cleavage of α-heteroaryl-substituted ...