Opportunities and Challenges in Applying Solid‐State NMR Spectroscopy in Organic Mechanochemistry DOI Creative Commons
Igor d’Anciães Almeida Silva, Ettore Bartalucci, Carsten Bolm

и другие.

Advanced Materials, Год журнала: 2023, Номер 35(52)

Опубликована: Июль 5, 2023

In recent years it is shown that mechanochemical strategies can be beneficial in directed conversions of organic compounds. Finding new reactions proved difficult, and due to the lack mechanistic understanding reaction events, respective efforts have mostly remained empirical. Spectroscopic techniques are crucial shedding light on these questions. this overview, opportunities challenges solid-state nuclear magnetic resonance (NMR) spectroscopy field mechanochemistry discussed. After a brief discussion basics high-resolution NMR under magic-angle spinning (MAS) conditions, seven for presented, ranging from ex situ approaches structurally elucidated products obtained by milling potential limitations approaches. Particular strengths NMR, instance differentiating polymorphs, NMR-crystallographic structure-determination protocols, or detecting weak noncovalent interactions molecular-recognition events employing proton-detected experiments at fast MAS frequencies,

Язык: Английский

Sustainability Assessment of Mechanochemistry by Using the Twelve Principles of Green Chemistry DOI
Karen J. Ardila‐Fierro, José G. Hernández

ChemSusChem, Год журнала: 2021, Номер 14(10), С. 2145 - 2162

Опубликована: Апрель 9, 2021

In recent years, mechanochemistry has been growing into a widely accepted alternative for chemical synthesis. addition to their efficiency and practicality, mechanochemical reactions are also recognized sustainability. The association between Green Chemistry often originates from the solvent-free nature of most protocols, which can reduce waste production. However, satisfies more than one Principles Chemistry. this Review we will present series examples that clearly illustrate how significantly contribute fulfillment in holistic manner.

Язык: Английский

Процитировано

466

Liquid‐Assisted Grinding Mechanochemistry in the Synthesis of Pharmaceuticals DOI

Ping Ying,

Jingbo Yu, Weike Su

и другие.

Advanced Synthesis & Catalysis, Год журнала: 2021, Номер 363(5), С. 1246 - 1271

Опубликована: Янв. 21, 2021

Abstract Mechanochemical reactions by milling, grinding or other types of mechanical action have emerged as a salient green approach because its wide applications towards academic and industrial chemical communities in sustainable solvent‐free/solvent‐less processes. Liquid‐assisted (LAG) an extension traditional solvent‐free mechanochemical techniques which small amount liquid is used additive to enhance and/or control reactivity, has been fruitfully applied the screening inclusion compounds, cocrystals, salts, solvates, polymorphs. However, utilization this important technique synthesis pharmaceutically biologically relevant targets was not adequately investigated. This review article summarizes overview latest development LAG approaches active pharmaceutical ingredients (API) drug‐like fragments, highlights superiority versus conventional syntheses. magnified image

Язык: Английский

Процитировано

250

Mechanochemistry: New Tools to Navigate the Uncharted Territory of “Impossible” Reactions DOI Creative Commons
Federico Cuccu, Lidia De Luca, Francesco Delogu

и другие.

ChemSusChem, Год журнала: 2022, Номер 15(17)

Опубликована: Июль 21, 2022

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 "thinking outside box", but also opened reaction paths, allowing overcome weaknesses traditional exactly where use well-established solution-based methodologies rules out progress. In this Review, reader is introduced an intriguing research subject not yet fully explored and waiting for improved understanding. Indeed, study mainly focused on that, although impossible solution, become possible under mechanochemical processing conditions, simultaneously entailing innovation expanding chemical space.

Язык: Английский

Процитировано

185

Tribochemistry, Mechanical Alloying, Mechanochemistry: What is in a Name? DOI Creative Commons
Adam A. L. Michalchuk∞, E.V. Boldyreva, Ana M. Belenguer

и другие.

Frontiers in Chemistry, Год журнала: 2021, Номер 9

Опубликована: Май 26, 2021

Over the decades, application of mechanical force to influence chemical reactions has been called by various names: mechanochemistry, tribochemistry, alloying, name but a few. The evolution these terms largely mirrored understanding field. But what is meant terms, why have they evolved, and does it really matter how process called? Which parameters should be defined describe unambiguously experimental conditions such that others can reproduce results, or allow meaningful comparison between processes explored under different conditions? Can information on encoded in clear, concise, self-explanatory way? We address questions this Opinion contribution, which we hope will spark timely constructive discussion across international mechanochemical community.

Язык: Английский

Процитировано

162

Continuous flow mechanochemistry: reactive extrusion as an enabling technology in organic synthesis DOI Creative Commons
Robert R. A. Bolt, Jamie A. Leitch, Andrew C. Jones

и другие.

Chemical Society Reviews, Год журнала: 2022, Номер 51(11), С. 4243 - 4260

Опубликована: Янв. 1, 2022

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

Язык: Английский

Процитировано

114

Green metrics in mechanochemistry DOI Creative Commons

Nicolas Fantozzi,

Jean‐Noël Volle, Andrea Porcheddu

и другие.

Chemical Society Reviews, Год журнала: 2023, Номер 52(19), С. 6680 - 6714

Опубликована: Янв. 1, 2023

The quantitative assessment of the greenness mechanochemical processes for green metrics were calculated is herein reported. A general introduction to topic, variables influencing reaction outcome and, an outlook are also provided.

Язык: Английский

Процитировано

87

Mechanochemistry Can Reduce Life Cycle Environmental Impacts of Manufacturing Active Pharmaceutical Ingredients DOI
Or Galant,

Giacomo Cerfeda,

Aaron S. McCalmont

и другие.

ACS Sustainable Chemistry & Engineering, Год журнала: 2022, Номер 10(4), С. 1430 - 1439

Опубликована: Янв. 20, 2022

The scale-up of mechanochemical methods could play a transformative role in making manufacturing processes the pharmaceutical industry greener by eliminating solvent use and recovery. Combined with energy-efficient continuous processing that consolidates reaction steps, mechanochemistry's environmental economic benefits may translate across product supply chains. Here, we evaluate numerous sustainability green chemistry metrics for producing nitrofurantoin, an active ingredient (API), via twin-screw extrusion (TSE) conventional solvent-batch synthesis methods. We find significant reduction all TSE including energy, climate change, human ecological health, as well cost due to reducing excess reactant consumption solvents while maintaining high selectivity. In addition, replacing direct energy source drive chemical from mostly thermal electrical sources does not increase net life cycle consumed produce functionally equivalent API. conclude holds multiple APIs potentially other products.

Язык: Английский

Процитировано

86

Salient Achievements in Synthetic Organic Chemistry Enabled by Mechanochemical Activation DOI
Eusebio Juaristi, C.G. Ávila-Ortíz

Synthesis, Год журнала: 2023, Номер 55(16), С. 2439 - 2459

Опубликована: Май 3, 2023

Abstract Although known for millennia, it is only recently that mechanochemistry has received serious attention by chemists. Indeed, during the past 15 years an extraordinary number of reports concerning solid-state chemical transformations through grinding and milling techniques have been recorded. This short review discusses circumstances led this renaissance, highlighting present intense interest in so-called green chemistry, enabling capacity to handle insoluble substrates, identification profound influence additives can on mechanochemically activated reactions. The core account focuses salient developments synthetic organic especially amino acid peptide­ mechanosynthesis, successful employment mechanochemical activation combination with asymmetric organocatalysis, promising enzymatic whole cell biocatalysis, remarkable achievement multicomponent selective reactions via complex, multistep reaction pathways, mechanosynthesis representative heterocycles. final section comments some pending tasks area, such as scaling-up processes be practical use industry, requirement easier more efficient control parameters monitoring devices, consequently careful analysis additional procedures a proper understanding phenomena. 1 Introduction 2 Brief History Mechanochemistry 3 Milling Equipment Reaction Parameters 4 Attributes That Propelled Its Present Renaissance 4.1 Enormous Attention Being Presently Paid Sustainable Chemistry 4.2 Reduced Energy Consumption 4.3 Additive-Based 4.4 Handling Insoluble Reactants 4.5 ‘Impossible’ Reactions Are Successful 4.6 Air- Water-Sensitive Reagents Ball 5 Salient Developments Mechanochemical Activation Synthetic Organic 5.1 Amino Acid Peptide Mechanosynthesis 5.2 Asymmetric Synthesis Organocatalysis under Ball-Milling Conditions 5.3 Mechanoenzymology 5.4 Multicomponent Activated 5.5 Heterocycles Modification 6 Future Directions 6.1 Scaling-Up Protocols 6.2 Temperature-Controlled 6.3 Understanding Transformations 6.4 Emerging Techniques 7 Conclusions

Язык: Английский

Процитировано

52

Tinkering with Mechanochemical Tools for Scale Up DOI Creative Commons
Javier F. Reynes, Valerio Isoni, Felipe Garcı́a

и другие.

Angewandte Chemie International Edition, Год журнала: 2023, Номер 62(44)

Опубликована: Апрель 28, 2023

Mechanochemistry provides an environmentally benign platform to develop more sustainable chemical processes by limiting raw materials, energy use, and waste generation while using physically smaller equipment. A continuously growing research community has steadily showcased examples of beneficial mechanochemistry applications at both the laboratory preparative scale. In contrast solution-based chemistry, mechanochemical have not yet been standardized, thus scaling up is still a nascent discipline. The purpose this Minireview highlight similarities, differences challenges various approaches that successfully applied for range scales. We hope provide discussion starting point those interested in further developing commercial use and/or industrialisation.

Язык: Английский

Процитировано

48

Upscaling Mechanochemistry: Challenges and Opportunities for Sustainable Industry DOI Creative Commons
Evelina Colacino, Valerio Isoni, Deborah E. Crawford

и другие.

Trends in Chemistry, Год журнала: 2021, Номер 3(5), С. 335 - 339

Опубликована: Март 27, 2021

Язык: Английский

Процитировано

105