Abstract Copolymerization of acrylonitrile (M1) with α-chloroacrylonitrile (M2) was carried out at 60 °C using 4.3×10−2 mol% of α,α′-azobisisobutyronitrile. The four copolymers obtained were analyzed, their mole fractions of α-chloroacrylonitrile units being 0.196, 0.377, 0.532, and 0.722, and the monomer reactivity ratios r1 and r2 were found to be 0.31 and 3.25, respectively.