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Functional high-entropy oxide (HEO) (Mg0.2Co0.2Ni0.2Cu0.2Zn0.2)O has attracted great attention due to its unique properties. High temperature (∼1000 °C) sintering is generally required to form the single-phase (Mg0.2Co0.2Ni0.2Cu0.2Zn0.2)O. In this work, a polyol process followed by quenching is established to synthesize (Mg0.2Co0.2Ni0.2Cu0.2Zn0.2)O. Benefiting from the homogeneous distribution of metal elements in the inorganic-organic hybrid compound obtained from polyol process, a single-phase HEO can be achieved after quenching at 800 °C.