Raman spectroscopy for real-time and in situ monitoring of mechanochemical milling reactions

Lukin, Stipe; Užarević, Krunoslav; Halász, Ivan

doi:10.1038/s41596-021-00545-x

Cited by 52 publications

(56 citation statements)

References 105 publications

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“…To get some insights into the mechanochemical reaction of 1c with NFSI we have performed in situ reaction monitoring of the milling process by Raman spectroscopy [ 32 – 33 ]. In an experiment milling 1c with NFSI (1 equiv) we observed the consumption of NFSI after ca.…”

Section: Resultsmentioning

confidence: 99%

Multi-faceted reactivity of N-fluorobenzenesulfonimide (NFSI) under mechanochemical conditions: fluorination, fluorodemethylation, sulfonylation, and amidation reactions

Hernández¹,

Ardila‐Fierro²,

Barišić³

et al. 2022

Beilstein J. Org. Chem.

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In the search for versatile reagents compatible with mechanochemical techniques, in this work we studied the reactivity of N-fluorobenzenesulfonimide (NFSI) by ball milling. We corroborated that, by mechanochemistry, NFSI can engage in a variety of reactions such as fluorinations, fluorodemethylations, sulfonylations, and amidations. In comparison to the protocols reported in solution, the mechanochemical reactions were accomplished in the absence of solvents, in short reaction times, and in yields comparable to or higher than their solvent-based counterparts.

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Section: Resultsmentioning

confidence: 99%

Multi-faceted reactivity of N-fluorobenzenesulfonimide (NFSI) under mechanochemical conditions: fluorination, fluorodemethylation, sulfonylation, and amidation reactions

Hernández¹,

Ardila‐Fierro²,

Barišić³

et al. 2022

Beilstein J. Org. Chem.

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show abstract

“…[52,57] Für eine ausführliche Diskussion der TRIS-Raman-Spektroskopie verweisen wir die Leser auf ein kürzlich veröffentlichtes Protokoll. [40] NMR-Spektroskopie. Ein neuer Ansatz zur Überwachung mechanochemischer Umwandlungen ist die Verwendung der zeitaufgelösten Festkörper-NMR (ssNMR).…”

Section: Methoden Für Die Direkte Analyseunclassified

Zeitaufgelöste In‐Situ‐Untersuchungen von mechanochemischen Reaktionen

Michalchuk

Emmerling

2022

Angewandte Chemie

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Mechanochemische Umwandlungen bieten umweltfreundliche Synthesewege und verbessern gleichzeitig die Geschwindigkeit und Selektivität von Reaktionen. Mechanochemie ermöglicht es, die Art und Weise, wie die Chemie in der Wissenschaft und in der Industrie betrieben wird, zu verändern, wird aber durch das mangelnde mechanistische Verständnis stark behindert. Die kontinuierliche Entwicklung und Anwendung von zeitaufgelösten In‐situ‐Methoden (time‐resolved in situ TRIS) zur Überwachung mechanochemischer Reaktionen bietet eine neue Dimension zur Erforschung dieser faszinierenden Umwandlungen. Wir diskutieren hier die jüngsten Trends in der Methodenentwicklung, die die Grenzen der mechanochemischen Forschung erweitert haben. Anschließend werden neue Merkmale mechanochemischer Reaktionen, die mit TRIS‐Techniken gewonnen wurden, erörtert, und es wird beleuchtet, wie verschiedene TRIS‐Ansätze verwendet wurden. Der Schwerpunkt liegt dabei auf der Stärke der Kombination komplementärer Techniken. Abschließend wird das Potenzial von TRIS‐Methoden in der mechanochemischen Forschung für die Etablierung eines neuen, umweltfreundlichen Paradigmas in den chemischen Wissenschaften dargestellt.

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“…To undoubtedly demonstrate and understand what is happening in a milling jar, mechanochemists have developed new tools for in situ monitoring. It is indeed possible to perform in situ PXRD with a modified vbm [25] or specially‐designed jars [26] inside a synchrotron, in situ solid‐state HR‐MAS NMR with a modified NMR probe, [27] as well as in situ Raman spectroscopy using transparent milling jars [28] . Hence, the number of in situ monitoring techniques is growing, but for the moment, if these techniques can complement each other and sometimes be used simultaneously, none of them can be universally applied to all mechanochemical systems.…”

Section: Equipmentmentioning

confidence: 99%

Sustainable Mechanosynthesis of Biologically Active Molecules

et al. 2022

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Synthetic mechanochemistry, the use of mechanical force produced by milling, grinding or extruding, as an activation technique, provides access to chemical entities of all kinds. This Review is focused on examples reported so far of known Active Pharmaceutical Ingredients (APIs), and effectively evaluated bioactive molecules, all prepared by mechanosynthesis. Three families of molecules are discussed: heterocyclic compounds, metal complexes and peptides. Advantages of the mechanochemistry approach are highlighted especially from a green chemistry and efficacy point of view.

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Raman spectroscopy for real-time and in situ monitoring of mechanochemical milling reactions

Cited by 52 publications

References 105 publications

Multi-faceted reactivity of N-fluorobenzenesulfonimide (NFSI) under mechanochemical conditions: fluorination, fluorodemethylation, sulfonylation, and amidation reactions

Multi-faceted reactivity of N-fluorobenzenesulfonimide (NFSI) under mechanochemical conditions: fluorination, fluorodemethylation, sulfonylation, and amidation reactions

Zeitaufgelöste In‐Situ‐Untersuchungen von mechanochemischen Reaktionen

Sustainable Mechanosynthesis of Biologically Active Molecules

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