Hydrogen atom transfer (HAT) chemistry has emerged as a powerful tool for selective molecular functionalization, with significant applications in the pharmaceutical and agricultural industries. More recently, HAT has been explored in polymer chemistry as a versatile strategy for introducing targeted functional groups onto polymer chains, enabling precise control over properties such as solubility and mechanical strength. This study investigates the use of HAT to synthesize reversible addition-fragmentation chain transfer (RAFT) agents (or chain transfer agents, CTAs) by modifying various substrates, including toluene, ethyl acetate, and dioxane, in the presence of bis(dodecylsulfanylthiocarbonyl) disulfide or bis(3,5-dimethyl-1