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Sr₂Fe_1.5Mo_0.5O_6−δ (SFMO) perovskite has been considered as a promising anode candidate for solid oxide fuel cells. However, the significant inconsistency in the conductivity properties of SFMO perovskite has been reported in the literature through various synthesis procedures, highlighting the necessity of a standard and unified synthesis process. In this work, we propose an optimized solid-state synthesis process of SFMO perovskite based on the thermal properties of the precursors. Our TG analysis indicates that the evaporation of MoO₃ during sintering over 752 °C may affect the synthesis of the expected SFMO perovskite. The presence of Fe₂O₃ has a trap effect on MoO₃, based on the TG analysis of the binary mixture. A cubically structured SFMO perovskite without a secondary phase is obtained from the as-proposed stepwise sintering program while an impurity phase of SrMoO₄ is observed when adopting a direct sintering program. The as-synthesized SFMO perovskite exhibits high stability in a reducing atmosphere, which is attributed to the self-adjustment of the overall valence states of molybdenum ions and iron ions. Many pure cubically structured perovskites have been successfully synthesized using the as-proposed solid-state synthesis process, suggesting its universality for the synthesis of other Mo-containing SOFC perovskite electrodes.