Continuous flow mechanochemistry: reactive extrusion as an enabling technology in organic synthesis

Bolt, Robert R. A.; Leitch, Jamie A.; Jones, Andrew C.; Nicholson, William I.; Browne, Duncan L.

doi:10.1039/d1cs00657f

Cited by 97 publications

(75 citation statements)

References 48 publications

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“…Looking into the future, one could expect that additional comparative studies between sonication and ball milling experiments will occur. At the same time, research into new modes to activate matter by force (e.g., twin-screw extrusion [71], resonant acoustic mixing [72], vortex fluidic mixing [73], laminar flow [74], etc.) will continue to unveil similarities and complementarities, rather than disparities, between the ways polymer and small molecule mechanochemical reactions occur.…”

Section: Discussionmentioning

confidence: 99%

Polymer and small molecule mechanochemistry: closer than ever

Hernández¹

2022

Beilstein J. Org. Chem.

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The formation and scission of chemical bonds facilitated by mechanical force (mechanochemistry) can be accomplished through various experimental strategies. Among them, ultrasonication of polymeric matrices and ball milling of reaction partners have become the two leading approaches to carry out polymer and small molecule mechanochemistry, respectively. Often, the methodological differences between these practical strategies seem to have created two seemingly distinct lines of thought within the field of mechanochemistry. However, in this Perspective article, the reader will encounter a series of studies in which some aspects believed to be inherently related to either polymer or small molecule mechanochemistry sometimes overlap, evidencing the connection between both approaches.

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Section: Discussionmentioning

confidence: 99%

Polymer and small molecule mechanochemistry: closer than ever

Hernández¹

2022

Beilstein J. Org. Chem.

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“…More recently, mechanochemical methods, including continuous flow mechanochemistry by TSE, for the preparation of APIs, have been quantitative assessed against the “12 Principles of Green Chemistry” by Colacino and co‐workers [14b] and in life cycle assessment studies (LCA) by Spatari and co‐workers [91] . A more detailed description of this technique and its applications in synthetic processes is available in a recent comprehensive Review article by Browne and co‐workers [195] …”

Section: Scale‐up: Twin‐screw Extrusionmentioning

confidence: 99%

“…[91] A more detailed description of this technique and its applications in synthetic processes is available in a recent comprehensive Review article by Browne and co-workers. [195]…”

Section: Scale-up: Twin-screw Extrusionmentioning

confidence: 99%

Mechanochemistry: New Tools to Navigate the Uncharted Territory of “Impossible” Reactions

et al. 2022

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Mechanochemical transformations have made chemists enter unknown territories, forcing a different chemistry perspective. While questioning or revisiting familiar concepts belonging to solution chemistry, mechanochemistry has broken new ground, especially in the panorama of organic synthesis. Not only does it foster new "thinking outside the box", but it also has opened new reaction paths, allowing to overcome the weaknesses of traditional chemistry exactly where the use of well-established solution-based methodologies rules out progress. In this Review, the reader is introduced to an intriguing research subject not yet fully explored and waiting for improved understanding. Indeed, the study is mainly focused on organic transformations that, although impossible in solution, become possible under mechanochemical processing conditions, simultaneously entailing innovation and expanding the chemical space.This publication is part of a joint Special Collection of Chemistry-Methods and ChemSusChem including invited contributions focusing on "Methods and Applications in Mechanochemistry". Please visit chemsuschem.org/ collections to view all contributions.

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“…This feature allows the intrinsic batch nature of ball milling, which hinders industrial scale-up, to be overcome (Calcio Gaudino et al, 2022). Extrusion is commonly applied in the polymer, materials and food industries while organic synthesis has only recently been investigated (Bolt et al, 2022), by means of new versatile single and twin screw micro-extruders.…”

Section: Ball Milling-mechanochemistry and Reactive Extrudersmentioning

confidence: 99%

Process intensification in continuous flow organic synthesis with enabling and hybrid technologies

et al. 2022

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Industrial organic synthesis is time and energy consuming, and generates substantial waste. Traditional conductive heating and mixing in batch reactors is no longer competitive with continuous-flow synthetic methods and enabling technologies that can strongly promote reaction kinetics. These advances lead to faster and simplified downstream processes with easier workup, purification and process scale-up. In the current Industry 4.0 revolution, new advances that are based on cyber-physical systems and artificial intelligence will be able to optimize and invigorate synthetic processes by connecting cascade reactors with continuous in-line monitoring and even predict solutions in case of unforeseen events. Alternative energy sources, such as dielectric and ohmic heating, ultrasound, hydrodynamic cavitation, reactive extruders and plasma have revolutionized standard procedures. So-called hybrid or hyphenated techniques, where the combination of two different energy sources often generates synergistic effects, are also worthy of mention. Herein, we report our consolidated experience of all of these alternative techniques.

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Continuous flow mechanochemistry: reactive extrusion as an enabling technology in organic synthesis

Abstract: Reactive extrusion provides a scale-up opportunity to turn a mechanochemical process from a ball-mill into continuous flow. This tutorial review summarises some of the early ground-breaking work in this area.

Cited by 97 publications

References 48 publications

Polymer and small molecule mechanochemistry: closer than ever

Polymer and small molecule mechanochemistry: closer than ever

Mechanochemistry: New Tools to Navigate the Uncharted Territory of “Impossible” Reactions

Process intensification in continuous flow organic synthesis with enabling and hybrid technologies

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