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Materials based on brush polymers are of great interest for study. Brush elastomers, obtained by grafting long side chains onto a linear backbone, exhibit a wide range of mechanical properties, such as the Young's modulus characteristic of gels with linear chains, and significant reversible deformations. The focus of this research is on brush block copolymers based on -butyl acrylate (PBA) and tert-butyl acrylate (PtBA), with degrees of polymerization for the side and main chains of 50 and 15, respectively. The synthesis of PtBA homopolymers with degrees of polymerization of 21, 50, 100, and 150 was carried out, as well as the synthesis of potassium methyl methacrylate (KOMA), which is necessary for converting the macroinitiator into a macromonomer, and the macromonomer PtBAso-MA, as well as a brush graft polymer based on them. Modern methods of physicochemical analysis were used to characterize the obtained compounds: gel permeation chromatography, NMR, and IR spectroscopy. Further studies of the physical properties of these polymers using synchrotron methods are planned.