Dynamics of phase separation in bisphenol-h polycarbonate (PC)/syndiotactic polymethyl methacrylate (sPMMA) blends has been investigated by means of time-resolved light scattering. Solvent-cast films of the PC/sPMMA blends were transparent, suggestive of miscible character. Several temperature jumps were carried out at a 50/50 PC/sPMMA composition from a homogeneous state (room temperature) into a two-phase regime. The process of phase separation first occurred for some considerable period, then it was followed by phase dissolution driven by chemical reaction. The thermodegradative reaction of sPMMA triggered the dissolution process by probably forming PC/sPMMA graft or random copolymers at the interface, which eventually resulted in a single phase. However, annealing at elevated temperatures for an extended period could lead to cross-linking, and thus a two-phase structure could be fixed permanently. The early stage of spinodal decomposition was interpreted in terms of the linearized Cahn-Hilliard theory. In the late stages of spinodal decomposition, the relationship between scattering peak wavenumber and time was found to obey a power law, but the exponents showed a strong dependence on temperature jumps. The temporal universal scaling failed due to the influence of the chemical reaction.