The production of molecules and materials enriched in stable isotopes is of major interest for different research fields. These compounds can for example be used (i) in analytical chemistry, to calibrate instruments and/or determine the structure of a new compound, and (ii) in synthetic chemistry, to elucidate reaction mechanisms. Yet, for elements like oxygen, which has three stable isotopes (99.76% ¹⁶O ; 0.04% ¹⁷O and 0.20% ¹⁸O), the ¹⁷O-labeling protocols available up until recently were generally unattractive, requiring long reaction times (up to several days/weeks), constraining experimental conditions (due to the use of air-sensitive or toxic reagents), and/or high costs (due to the use of large excesses of expensive enriched precursors). In this context, our research group has been focussing on developing more efficient ¹⁷O-labeling strategies using ball-milling. In this presentation, we will present an overview of different strategies we have developed for enriching a variety of organic molecules and inorganic compounds in ¹⁷O,^[1] and we will illustrate how these newly-enriched species can be used for high-resolution ¹⁷O NMR analyses.^[2]
[1] (a) J. Špačková, C. Fabra, G. Cazals, M. Hubert-Roux, I. Schmitz-Afonso, I. Goldberga, D. Berthomieu, A. Lebrun, T.-X. Métro, D. Laurencin, Chem. Commun. 2021, 57, 6812 ; (b) C.-H. Chen, E. Gaillard, F. Mentink-Vigier, K. Chen, Z. Gan, P. Gaveau, B. Rebière, R. Berthelot, P. Florian, C. Bonhomme, Mark E. Smith, T.-X. Métro, B. Alonso, D. Laurencin, Inorg. Chem. 2020, 18, 13080 ; (c) T.-X. Métro, C. Gervais, A. Martinez, C. Bonhomme, D. Laurencin, Angew. Chem. 2017, 56, 6803.
[2] (a) I. Goldberga, N. Patrix, C.-H. Chen, E. Thomassot, J. Trébosc, I. Hung, Z. Gan, D. Berthomieu, T.-X. Métro, C. Bonhomme, C. Gervais, D. Laurencin, J. Phys. Chem. C, 2022, 126, 12044 ; (b) C. Leroy, T.-X. Métro, I. Hung, Z. Gan, C. Gervais, D. Laurencin, Chem. Mater., 2022, 34, 2292 ; (c) J. Špačková, C. Fabra, S. Mittelette, E. Gaillard, C.-H. Chen, G. Cazals, A. Lebrun, S. Sene, D. Berthomieu, K. Chen, Z. Gan, C. Gervais, T-X. Métro, D. Laurencin, J. Am. Chem. Soc. 2020, 142, 21068.

Danielle Laurencin

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