Combined self-propagating high-temperature synthesis and hydride cycling methods form a novel and recently developed technique allowing preparing specific multiple-phase materials. Ternary Laves phase related to bcc solid solution and binary bcc V–Ti alloys and their hydrides were prepared using this route. In this report, the microstructure and hydrogenation properties of V–Ti alloys were investigated as well as hydrogenation of the phase transitions in the Ti–V–H systems. It was found that hydrogen evacuates from the compounds via a single step. The typical temperature of phase transformation depends weakly on the composition of the alloys.