The short-chain epoxy resin (SCER) was prepared direct from epichlorohydrin/bisphenol A (ECH/BPA). The resulted SCER and 4,4'-diaminodiphenyl sulfone (DDS) with various weight percent of triallyl isocyanurate/4,4'-bismaleimidophenytmethane (TAIC/BMI) were subsequently thermally coreacted to the corresponding high performance materials for high frequency application. They were characterized using potentiometry, Fourier transform infrared (FTIR), differential scanning calorimetry (DSC), thermogravimetric analyses (TGA), dielectric analyzer, and scanning electron microscope (SEM). Dynamic mechanical analysis (DMA) of polymers showed only a T-g indicating a low entropy, amorphous state and formed a conterminously linked polymer. The morphology of polymers revealed no phase separation. The formation of polymer was in good agreement with the proposed molecular structure, and has enhanced good thermal, mechanical, and electric properties. Furthermore, with lower nitrogen content was achieved UL94 V-0 rating. No fume and toxic gas emission were observed during burning test for this system. (c) 2006 Wiley Periodicals, Inc.