Onkarappa, S.B.Bhat, N.S.Dutta, S.2026-02-052020Biomass Conversion and Biorefinery, 2020, 10, 4, pp. 849-85621906815https://doi.org/10.1007/s13399-020-00791-1https://idr.nitk.ac.in/handle/123456789/23587This work reports the synthesis of a series of alkyl levulinates from biomass-derived 5-(halomethyl)furfural (X = Cl, Br), furfuryl alcohol, and angelica lactone using silica-supported perchloric acid (HClO<inf>4</inf>-SiO<inf>2</inf>) as a heterogeneous acid catalyst. The solvent-free, one-pot preparation afforded levulinate esters in excellent isolated yields (> 84%). The reactions were performed at 120 °C for 6 h in a batch-type glass pressure reactor using XMF and furfuryl alcohol in presence of excess of the alcohol reagent and 4 wt.% of the HClO<inf>4</inf>-SiO<inf>2</inf> catalyst (0.028 mmol HClO<inf>4</inf>). Furthermore, the reaction protocol was extended for the synthesis of ALs starting with angelica lactone at 90 °C for 2 h in a round-bottomed flask by using excess alcohol and 4 wt.% of the HClO<inf>4</inf>-SiO<inf>2</inf> catalyst. © 2020, Springer-Verlag GmbH Germany, part of Springer Nature.AldehydesCatalystsEstersFurfuralInorganic acidsSilicaSiliconFurfuryl alcoholHeterogeneous acid catalystsIsolated yieldOne-pot preparationsPerchloric acidsPressure reactorsReaction protocolsSolvent freeChlorine compounds