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Poster De Conférence Année : 2022

Understanding the Mechanochemical Synthesis of [Cu(Cl)(NHC)] Complexes using Solid-State NMR Spectroscopy


The use of solvents in modern synthesis has now reached enormous quantities and with the aim of reducing the footprint of synthesis, the use of solvents needs to be reduced or, even better, eliminated. Mechanochemistry is one possible route to achieve this goal. Nevertheless, several reaction mechanisms involved in mechanochemistry are still elusive. As a local characterization technique endowed with atomic resolution, solid-state NMR spectroscopy represents a promising method to unveil the mechanism of mechanosynthesis. Recently we applied solid-state NMR to study the mechanochemical synthesis of transition metal complexes bearing N-heterocyclic carbene (NHC) ligands with applications in catalysis and anti-infective coatings in medical devices.1,2,3 In particular, we investigated the effect of the successive work-up protocols for the preparation of [Cu(Cl)(NHC)] complexes. This compound was prepared under ball milling and solvent-free conditions in two different ways, (i) one-pot synthesis and (ii) step-wise synthesis. Multinuclear ( 1H, 13C, 15N, 35Cl, and 63Cu) solid-state NMR experiments at 9.4 and 18.8 T were conducted to monitor the consumption of the reactants and the formation of the intermediate and final product for the different synthetic routes and work-up protocols. NMR signals were assigned with the help of 2D heteronuclear correlation as well as DFT calculations of NMR parameters. The NMR signals of 13C nucleus bonded to 63,65Cu isotope in [Cu(Cl)(NHC)] complex exhibits multiplet due to J-coupling and quadrupolar-dipolar cross-term. In this presentation, we will show the results ofthese experiments and the notable differences we observe between the one-pot and stepwise processes.


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Dates et versions

hal-04347405 , version 1 (15-12-2023)



  • HAL Id : hal-04347405 , version 1


Lama Hamdouna, Gianmarco Pisano, Andrew G. M. Rankin, Laura Falivene, Julien Trebosc, et al.. Understanding the Mechanochemical Synthesis of [Cu(Cl)(NHC)] Complexes using Solid-State NMR Spectroscopy. 61st Annual Rocky Mountain Conference on Magnetic Resonance, solid-state NMR symposium, Jul 2022, Copper Mountain, United States. Digital Commons, Final program and abstracts, 428, pp.145-146, 2022. ⟨hal-04347405⟩
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