Synthesis of segmentally deuterated poly(acetyliminoethylene) lipopolymers, material for neutron scattering and NMR studies

We describe the synthesis of lipopolymers suitable for conformation and mobility studies by neutron scattering methods and 2H-NMR spectroscopy. Starting with 2-methyl-2-oxazoline MeOx monomers, we developed two synthetic routes for the preparation of 2-trideuteromethyl-2-oxazoline D3-MeOx. Both rely on cheap and easily available deuterated sources, but the yield of the products and their degree of deuteration as well as efficiency differ considerably. Using a lipid initiator, we efficiently introduced the lipid end-group into the polymer. Sequential addition of deuterated and non-deuterated monomers led to the segmentally deuterated poly(acetyliminoethylene) lipopolymers [diblock or triblock copolymers consisting of poly(acetyliminoethylene) and poly(trideuteroacetyliminoethylene)]. We also achieved good control of the position and length of the blocks with a narrow molecular mass distribution. Two sets of substances were synthesized differing in molecular mass and degree of deuteration. The physical properties of these substances are described separately.