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Item Hydrochloric acid-catalyzed coproduction of furfural and 5-(chloromethyl)furfural assisted by a phase transfer catalyst(Elsevier Ltd, 2020) Bhat, N.S.; Vinod, N.; Onkarappa, S.B.; Dutta, S.Furfural has been produced in 53% isolated yield from D-xylose within an aqueous HCl-1,2-dichloroethane biphasic reaction mixture using benzyltributylammonium chloride (BTBAC) as a phase transfer catalyst. The use of BTBAC noticeably improved the yield of furfural compared to that in the control reaction. The reaction was optimized on the reaction temperature, duration, concentration of HCl, and the loading of BTBAC. Furfural and 5-(chloromethyl)furfural (CMF) have also been coproduced from a mixture of pentose and hexose sugars. Under optimized conditions (100 °C, 3 h, 20.2% HCl, 10 wt% BTBAC), CMF and furfural were isolated in 17% and 53% yield, respectively, from a mixture of glucose and xylose. In addition, levulinic acid was isolated from the aqueous layer in 31% yield. © 2020 Elsevier LtdItem Preparation of alkyl levulinates from biomass-derived 5-(halomethyl)furfural (X = Cl, Br), furfuryl alcohol, and angelica lactone using silica-supported perchloric acid as a heterogeneous acid catalyst(Springer Science and Business Media Deutschland GmbH, 2020) Onkarappa, S.B.; Bhat, N.S.; Dutta, S.This 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 (HClO4-SiO2) 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 HClO4-SiO2 catalyst (0.028 mmol HClO4). 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 HClO4-SiO2 catalyst. © 2020, Springer-Verlag GmbH Germany, part of Springer Nature.
