The biofuel chemicals, 5-ethoxymethylfufural (EMF) and 5-methoxymethylfufural (MMF) have been prepared from various carbohydrates in alcoholic solvents. The porous polymeric material PSDVB-SO 3 H was employed as a heterogeneous catalyst in this investigation and the reaction parameters; time, temperature, catalyst/feedstock loading and co-solvent were optimized. As a result of the acid density and mesoporous structure, PSDVB-SO 3 H efficiently catalyzed the ethanolysis of fructose to EMF in a 67.5% yield (2 h, 393 K). Whereas MMF was obtained in a 31.6% yield from the catalytic methanolysis of fructose. Compared to commercial Amberlyst-15, less time was required for PSDVB-SO 3 H to obtain a comparable yield of EMF. Alkyl levulinates and 5-hydroxymethylfurfural (HMF) were the main co-products in these reactions, with yields in the range of 0–67% obtained from the catalytic alcoholysis of fructose. Furthermore, by using a "two-step, one-pot" route with successive addition of zeolite zeolite and PSDVB-SO 3 H to a solution of glucose, EMF was achieved in a yield of 39.4%. • An efficient reaction system for producing EMF/MMF was proposed. • Ethanolysis of fructose to EMF with a yield of 67.5% was achieved. • The combination of zeolite and PSDVB-SO 3 H facilitated glucose conversion to EMF/MMF. • EL and ML were the main co-products, with yields in the range of 0–67% obtained. • Both acidity and textural structure of the catalyst played an important role. [ABSTRACT FROM AUTHOR]