5-Hydroxymethylfurfural (HMF) was synthesized from monosaccharides by a biphasic reaction system using a microreactor. The biphasic reaction system realized an immediate extraction and stabilization of product HMF, which further degrades under the reaction conditions. Segmented flow was utilized for an efficient reaction-extraction tool. The effect of extraction ability was evaluated based on the extraction phase/reaction phase partition coefficient of HMF. A Lewis acid catalyst was introduced to overcome the obstacle of the reaction, which was clarified as the isomerization of glucose to fructose, and improved the HMF yield to 85 mol % under the condition of T = 180 °C and τ = 47 min. The recovery of the product HMF was also examined using a constructed microextraction system, and HMF was selectively recovered from the extraction phase.
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