Summary
Two novel ATRP initiator (R‐X): 2‐bromo‐2‐methyl‐N‐(1‐phenyl‐ethyl)propanamide (I) and 2,2,2‐trichloro‐N‐(1‐phenylethyl)acetamide (II) were synthesized and characterized by 1H‐NMR, IR, EI. Also, crystal structures of (I) and (II) are reported. Compounds (I) and (II) were used in the ATRP reaction of methyl methacrylate (MMA) and acrylamide (AAD) at 48°C, using CuBr/Me6TREN and ethanol/toluene (60:40) mixture as catalytic complex and solvent, respectively. End‐group analysis by 1H‐NMR was used to determinate the molecular mass of the polymers synthesized via ATRP. The Mn values for poly(MMA) using (II) were 2333 and 3952 g/mol, which is higher in comparison with the Mn values obatined for (AAD)/(II) and (AAD)/(I) systems indicating that monomers containing ester moiety in their structure, such as acrylates and methacrylates, may be good candidates to polymerize with (II) and CuBr/Me6TREN.