Issue 13, 2022

Continuous flow Meerwein–Ponndorf–Verley reduction of HMF and furfural using basic zirconium carbonate

Abstract

Continuous Flow Microreactors and Green Chemistry are areas with promising applications, especially when allied. In this scenario, the main goal of this study was to develop new strategies for the synthesis of bio-based compounds under a flow regime. We worked towards the flow synthesis of furfuryl alcohol and DHMF (dihydroxymethylfuran), from their respective aldehydes, through a Meerwein–Ponndorf–Verley reaction with iso-propanol catalysed by basic zirconium carbonate. Furfuryl alcohol was prepared in essentially quantitative yield with productivities as high as 67 mg min−1. Efforts towards DHMF synthesis were performed and the process was also optimized using design of experiments. The optimal conditions were defined for DHMF at 0.25 M and were determined to be 120 °C and 50 s of residence time, giving yields of up to 99% and productivity of 50 mg min−1. The use of a FT-IR device for the in-line continuous monitoring was pivotal for the fast optimization of the processes, securing steady-state operations, and design of experiments ensured a greater understanding of the effect of temperature, residence time and concentration, alongside their interactions in yield, selectivity and productivity.

Graphical abstract: Continuous flow Meerwein–Ponndorf–Verley reduction of HMF and furfural using basic zirconium carbonate

Supplementary files

Article information

Article type
Paper
Submitted
27 jan 2022
Accepted
04 mar 2022
First published
11 mar 2022
This article is Open Access
Creative Commons BY-NC license

RSC Adv., 2022,12, 7980-7989

Continuous flow Meerwein–Ponndorf–Verley reduction of HMF and furfural using basic zirconium carbonate

H. M. Marçon and J. C. Pastre, RSC Adv., 2022, 12, 7980 DOI: 10.1039/D2RA00588C

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