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Cyclohexene esterification–hydrogenation for the efficient production of cyclohexanol will be commercialized for the first time. Cu/MgO/Al₂O₃ catalysts with layered double hydroxides as precursors were developed, and the effect of altering the reduction temperature on the catalytic activity was explored. Fresh and spent Cu/MgO/Al₂O₃ catalysts exhibited excellent catalytic performance after thermal treatment during the hydrogenation of cyclohexyl acetate to cyclohexanol. STEM images showed that the Cu particles grew slightly, without obvious aggregation. Based on the results of XAES and in situ FTIR of the adsorbed CO method, optimal performance (conversion rate of 99.59% with 98.94% selectivity) was achieved, which was attributed to the synergistic effect on the surface-active Cu⁰ and Cu⁺ sites with Cu⁰/(Cu⁰ + Cu⁺) of around 0.70, and the ratios could be maintained at temperatures of 513–553 K. The morphology of Cu/MgO/Al₂O₃ catalysts was well preserved during the hydrogenation of cyclohexyl acetate, indicating potential industrial applications. The well-dispersed Cu/MgO/Al₂O₃ catalyst with a stable microstructure possesses an adjustable valence state and thermal stability during the hydrogenation of cyclohexyl acetate, giving it industrial application prospects.