The copolymerization of vinyl acetate with methyl acrylate in the presence of Et2AlCl, Et1.5AlCl1.5, and Et2AlCl‐benzoyl peroxide systems has been investigated. The influence of monomer ratios and organoaluminium compound concentration on the copolymer yield and composition have been determined and discussed. The monomer sequences distribution has been studied by means of 13C‐NMR. It was found that organoaluminium compounds in the studied systems catalyze not only the alternating copolymerization, but also the homopropagation of both monomers. An alternating copolymer was obtained in reactions carried out at −78°C, when a large excess of vinyl acetate was used in the monomer feed.
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