Autonomous reaction self-optimization using in-line high-field NMR spectroscopy - Archive ouverte HAL Accéder directement au contenu
Article Dans Une Revue Reaction Chemistry & Engineering Année : 2024

Autonomous reaction self-optimization using in-line high-field NMR spectroscopy

Résumé

Automated self-optimization in flow is a powerful approach to efficiently optimize chemical transformations in a high dimensional space. Self-optimizing flow reactors combine automated flow devices with feedback optimization algorithms, which are powered by process analytical technology. In this contribution we introduce the concept of autonomous self-optimizing flow reactors guided by in-line high-field NMR spectroscopy. We designed an autonomous experimental setup, combining an automated flow reactor with a high-field NMR spectrometer and a feedback optimization algorithm. User-friendly interfaces were developed for straightforward input of experimental parameters and precise control of equipment. Using 1D 1H NMR spectroscopy with a solvent suppression method, we achieved accurate quantitative measurements. A self-optimization utilizing the Nelder-Mead algorithm to maximize either the yield or the throughput of a formal [3 + 3] cycloaddition was conducted through the fine-tuning of the residence time, stoichiometry, and catalyst loading as input variables. The integration of high-field NMR within autonomous flow systems promises enhanced precision, and efficiency in chemical synthesis optimization, particularly for complex reaction mixtures, setting the stage for advances in chemical synthesis.
Fichier sous embargo
Fichier sous embargo
0 5 11
Année Mois Jours
Avant la publication
dimanche 29 décembre 2024
Fichier sous embargo
dimanche 29 décembre 2024
Connectez-vous pour demander l'accès au fichier

Dates et versions

hal-04637947 , version 1 (08-07-2024)

Licence

Copyright (Tous droits réservés)

Identifiants

Citer

Nour El Sabbagh, Margherita Bazzoni, Yuliia Horbenko, Aurélie Bernard, Daniel Cortés-Borda, et al.. Autonomous reaction self-optimization using in-line high-field NMR spectroscopy. Reaction Chemistry & Engineering, In press, ⟨10.1039/D4RE00270A⟩. ⟨hal-04637947⟩
0 Consultations
0 Téléchargements

Altmetric

Partager

Gmail Mastodon Facebook X LinkedIn More