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Furan derivatives obtained from renewable biomass resources have the potential to serve as substitutes for the petroleum-based building blocks that are currently used in the production of plastics and fine chemicals. We developed a process for the selective dehydration of fructose to 5-hydroxymethylfurfural (HMF) that operates at high fructose concentrations (10 to 50 weight %), achieves high yields (80% HMF selectivity at 90% fructose conversion), and delivers HMF in a separation-friendly solvent. In a two-phase reactor system, fructose is dehydrated in the aqueous phase with the use of an acid catalyst (hydrochloric acid or an acidic ion-exchange resin) with dimethylsulfoxide and/or poly(1-vinyl-2-pyrrolidinone) added to suppress undesired side reactions. The HMF product is continuously extracted into an organic phase (methylisobutylketone) modified with 2-butanol to enhance partitioning from the reactive aqueous solution.