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Thermal-chemical pre-treatment has proven to facilitate the solubilization of organics and improvement in biogas generation from the organic fraction of municipal solid waste (OFMSW). However, the production of recalcitrant is inevitable when OFMSW is pretreated at high temperatures and alkali dosage. This study develops a strategy to use Fe³⁺ to reduce the formation of recalcitrant compounds, i.e., 5-HydroxyMethyl Furfural (5-HMF), furfurals, and humic acids (HA) during thermal-alkali pre-treatment. It was postulated that the formation of the recalcitrant compound during pre-treatment can be reduced by Fe³⁺ dosing to oxidize intermediates of Maillard reactions. A decrease in 5-HMF (45–49%) and furfurals (54–66%) was observed during Fe³⁺ (optimum dose: 10 mg/L) mediated thermal-alkali pre-treatment owing to the Lewis acid behavior of FeCl₃. The Fe³⁺ mediated assays show a substantial improvement …