Alkoxide sol-gel processing of Y1Ba2Cu3O7-x was performed using copper(II) ethoxide, barium methoxyethoxide, and yttrium methoxyethoxide precursors in a methoxyethanol/methy ethyl ketone/toluene solvent system. In situ neutron diffraction experiments were performed on individual precursors and mixed component gels during heat treatment. Phase development and consumption was observed for both the calcination and annealing segments of the heat treatment. Formation of Y1Ba2Cu3O7-x was observed as early as 700°C. CuO, Cu2O, BaCuO, YCu2O5, BaCO3, BaCO4, and YlBa2Cu3O7-x were observed during the conversion/ consolidation reactions to 850°C.