Abstract The conversion of fructose into 2,5‐diformylfuran (DFF) is a tandem reaction that consists of the dehydration of fructose to 5‐hydroxymethylfurfural (HMF) catalyzed by an acid catalyst and subsequent oxidation of HMF to DFF by a redox catalyst. Phosphomolybdic acid encapsulated in MIL‐101 (PMA–MIL‐101), with high Brønsted acidity and moderate redox potential, was evaluated as a promising catalyst for the one‐pot synthesis of DFF directly from fructose. The results demonstrated that PMA–MIL‐101 was an efficient and recyclable bifunctional catalyst for the production of DFF from fructose in DMSO; it showed high activity and selectivity towards the direct transformation of fructose into DFF, and it could be reused. A satisfactory DFF yield of 75.1 % was obtained over 2 PMA–MIL‐101 in a one‐pot, one‐step reaction under optimal reaction conditions.