<正> The 1H NMR spectra recorded during the thermolysis of lauroyl peroxide and of 3,5,5-trimethylhexanoyl peroxide in ODCB containing 2-iodopropane show CIDNP multiplet effect. It wasobserved that the relative concentrations of 1-iodoundecane and 2-iodopropane. both polarized andnormal species. changed with time. The relaxation time T1 of the a-protons in 1-iodoundecaneand vinyl protons of CH2 in 1-undecene, enhancement factor of the protons of polarized species andthe rate constant of decomposition for lauroyl peroxide have been determined. The mechanismof the decomposition of the entitled peroxides is discussed in terms of the radical pair theory.