Levulinic acid and angelica lactones are important building blocks obtained from hemicellulose. This process comprises multiple chemical reactions at which furfuryl alcohol is an intermediate, but only few studies have investigated its hydrolysis. This work studied the role played by the nature of acid sites and the impact of their strength and amount on furfuryl alcohol hydrolysis over Nb2O5 and NbOPO4. It was disclosed that production of levulinic acid is a two‐step cascade reaction at which angelica lactones are intermediates. These two hydrolysis steps were catalyzed by Brønsted acid sites with no contribution from Lewis centers. Brønsted acidity of Nb2O5 presented no activity while phosphate moieties on NbOPO4 were effective. Mixtures of organic solvent and water hindered side reactions, improving selectivity to valued bioproducts. 1,4‐dioxane was the most suitable organic solvent. This study shows that selectivity of 96 % of levulinic acid and angelica lactones can be accomplished over NbOPO4.

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