Scalable Mechanochemical Synthesis of Amides Using Bead Milling Technology
Amide bonds are among the most ubiquitous linkages in pharmaceuticals, agrochemicals, and materials, yet their synthesis is still dominated by solvent-intensive protocols. Mechanochemistry offers a sustainable alternative, but its scalability has remained a critical challenge. Here we demonstrate that amide bond formation can be translated into an industrially relevant process using a standard agitator bead mill. Through systematic optimization, we achieved efficient amidations over a broad substrate scope under liquid-assisted grinding with only minimal ethyl acetate. A 20-fold scale-up delivered productivities of up to 2.89 kg/h, without excess reagents, added base, or bulk solvent, substantially reducing waste. The use of a commercially available equipment that is available from lab to manufacturing-scale establishes bead milling as a practical, scalable, and environmentally responsible platform for scalable amide synthesis.
Authors
- Sándor B. Ötvös (ORCID: https://orcid.org/0000-0001-6673-1744)
- Andrea Porcheddu (ORCID: https://orcid.org/0000-0001-7367-1102)
- C. Oliver Kappe (ORCID: https://orcid.org/0000-0003-2983-6007)
- Pietro Caboni (ORCID: https://orcid.org/0000-0002-7507-4974)
Institutions
- University of Graz (AT)
- University of Cagliari (IT)
- Istituto Nazionale di Fisica Nucleare, Sezione di Cagliari (IT)
- Research Center Pharmaceutical Engineering (Austria) (AT)
Publication Details
- Journal
- ChemRxiv
- Published
- 2025-09-15
- DOI
- https://doi.org/10.26434/chemrxiv-2025-40n7x
- Primary Topic
- Chemical Synthesis and Analysis
- Type
- article
- Field-Weighted Citation Impact
- 0.00
Funders
- Royal College of Physicians of Edinburgh
- Bundesministerium für Digitalisierung und Wirtschaftsstandort