Abstract: | Imine macrocycle M1 was successfully used in conjunction with CuBr as a catalytic system in the atom transfer radical polymerization (ATRP) of methyl methacrylate (MMA). The role of the reaction conditions was clearly observed. Such reaction conditions were found to be the molar ratios of the reactants, the chosen initiating systems, and some additional ambient conditions (e.g. temperature, solvent). MMA homopolymers were successively prepared via ATRP by using benzhydrylbromide, diethylmethylbromomalonate initiating systems under the appropriate reaction conditions. Definite well‐known structures of the formed polymers were unambiguously identified with 1H NMR. |