Notably, P1 was produced over 90% yield on a 100-gram scale, indicating the practicality of this method (Figure ). We further explored the generality of GTRP The refinement of conditions for the copolymerization of 2-phenyl hexenenitrile M13 and acrylonitrile was performed using azobisisoheptanenitrile (ABVN) as an initiator at 75 °C across an array of solvents including N-methylpyrrolidone (NMP), DMSO, DMF, and chlorobenzene (PhCl), and culminated in the synthesis of copolymers exhibiting narrowly dispersity values (1.18-1.22) compared to homopolymerization process (Table , entries 1-4). It was observed that solvent had little impact on the Mn and Đ of the resulting copolymers. Conversely, the substitution of ABVN with other initiators like AIBN, benzoyl peroxide (BPO), and tert-butyl peroxide (TBPB) resulted in suboptimal monomer conversion rates (Table , entries 5-7). The GTRP copolymerization process yielded a light-yellow solid product, demonstrating solubility in dichloromethane (DCM) and the miscibility with polar solvents such as DMF and DMSO. An intriguing structural attribute of the resulting copolymers was the formation of an ABB sequence when a slight excess of 2-phenyl hexenenitrile was present. The chain structure of the copolymer was confirmed using 1 H and C NMR spectroscopy (Figure ). Extending our attempts to alternative monomers such as acrylic ester and acrylamide were trialed, yet these efforts culminated in the generation of random copolymers so far. Entry Initiator Solvent Yield (%) Mn (kg•mol -1 ) [c] initiator (2 mol %), in a 4 mL vial under N2 for 24 h at 70 º C. Yields of isolated product after precipitation with methanol (10 mL). Molecular weight and dispersity were determined by GPC in DMF with polystyrene as an internal standard at 50 º C, LiBr/DMF solution (0.01 mol L -1 ) was used as the mobile phase. Initiator (4 mol %). 75 º C.