Dehydration of fructose to 5-Hydroxymethylfurfural with ZrCl4Dehydration of fructose to 5-Hydroxymethylfurfural with ZrCl4
SyntheticPage 769
Published Nov 24, 2014
Solution containing D-Fructose (1 g, 5.55mmol) in nitromethane (10mL) was charged into a 50 mL flask, followed by the addition of ZrCl4 (0.129 g, 0.55mmol).The mixture was then heated at 1000C for 3 h, while stirred with a magnetic stirrer. Reaction mixture was cooled to rt and evaporated under reduced pressure to get crude mass, which was diluted with water (25 mL) and extracted with ethyl acetate (50 mL×4).After drying on Na2SO4 extracts were concentrated on rotatory evaporator. Purification by column chromatography (80-20% ethyl acetate in petroleum ether as eluent) to gave 5-Hydroxymethylfurfural (0.52g, yellow oil, yield:73%).