Cryotachensic copolymerization of chloral with various aliphatic and aromatic isocyanates, initiated by lithium tert-butoxide and triphenylphosphine at O"C, was followed by 'H NMR spectroscopy. Information on the mobility of comonomers and solvent molecules in the polymerization mixture was obtained by measuring the line width of the signals. Relative rates of incorporation of chloral and isocyanates into the copolymer were determined, indicating that the copolymer was not uniform in structure and that the content of isocyanate units increased significantly in the final stages of copolymerization.