The subsequent experiments involved examining various reagent ratios. Increasing the amount of benzoic acid hampered functionalization (21% conv., entry 5). Adding more TBAI catalyst had a slight impact, resulting in 83% conv. (0.20 equiv., entry 6) and 72% conv. (0.30 equiv., entry 7). Doubling all reagents except PEO decreased efficiency and increased chain deterioration (61% conv., Ð = 1.36, entry 8). The progress of the reaction was monitored over time (entries 2, 9, and 10). Both C-H functionalization and chain alteration proceeded consistently. Once benzoic acid was mostly consumed, chain damage became a significant process, leading to a broader chain length dispersity (92% conv., Ð = 1.41, entry 11). A series of experiments was conducted on a longer chain, PEO 20K (Mn = 19.6 Kg/mol) (Table ). The reactivity remained unchanged, but there was an enhancement in the degree of dispersity broadening. Although chain scission may have occurred at the same rate, it was more frequent per chain compared to PEO 6K. Under the same conditions as entry 2 of Table , a significant increase in dispersity was observed, resulting in a value of 1.42 (entry 1). However, by reducing TBHP to 0.5 equiv., a narrow dispersity was restored (entries 2 and 3), and the efficiency of PPM was improved by increasing TBAI (67%, entry 3).