The synthesis of bis(thiophenol-F) glycidyl methacrylate (BIS-GMTF) by the addition reaction between epoxide resin and methacrylic acid is described. The reaction was carried out without a solvent (in the alloy) and with the solvent (xylene). The reaction kinetics between the epoxide and carboxyl group during the BIS-GMTF reaction was observed by chemical analytical methods and infrared radiation (IR). The esterification is a second-order reaction at temperatures >45degreesC in the alloy and 70degreesC in the solvent. The spectroscopic characteristics of unsaturated BIS-GMTF resin were determined from IR, H-1-NMR, and C-13-NMR spectra. Epoxymethacrylate was subjected to photocuring, with the addition of IRGACURE 651, with a high-pressure mercury lamp in an oxygen-free atmosphere. The cured foil was subjected to thermal, thermomechanical, and mechanical investigations.