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

Institutions

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

Controls
|||
ALL TIME
JAN
FEB
MAR
APR
MAY
JUN
JUL
AUG
SEP
OCT
article

Scalable Mechanochemical Synthesis of Amides Using Bead Milling Technology

Sándor B. Ötvös, Andrea Porcheddu, C. Oliver Kappe, Pietro Caboni
ChemRxiv
Chemical Synthesis and Analysis
article

Scalable Mechanochemical Synthesis of Amides Using Bead Milling Technology

Sándor B. Ötvös, Andrea Porcheddu, C. Oliver Kappe, Pietro Caboni
article en

Abstract

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.

ChemRxiv
University of Graz (AT), University of Cagliari (IT), Istituto Nazionale di Fisica Nucleare, Sezione di Cagliari (IT), Research Center Pharmaceutical Engineering (Austria) (AT)
Royal College of Physicians of Edinburgh, Bundesministerium für Digitalisierung und Wirtschaftsstandort
Openalex Percentile: Top 78%
Chemical Synthesis and Analysis
AI Navigator

Ask Laika to Summarize, Analyze, and Connect papers live on the map.

Summarize Papers & Methodologies

Extract key findings, datasets, and comparative methods across publications.

Benchmark Rankings & Visual Analytics

Rank top research institutions, authors, funders, topics, and journals by Field-Weighted Citation Impact (FWCI) and paper volume with instant charts.

Connect Distant Disciplines

Bridge topological clusters on the map to find hidden collaborative intersections.