"Quantitative in-situ NMR-Illumination for Excitation and Kinetic Analysis of Molecular Motor Intermediates"R. Wilcken, A. Gerwien, L. Huber, H. Dube, and E. Riedle
ChemPhotoChem 6, e202100232 (2022).
Modern synthetic methods can be highly complex and proceed via multiple sequential processes. The intricate concepts can rarely be checked in all details due to the lack of suitable analysis methods. For photo-initiated reactions the starting point can be chosen to any desired precision by short or ultrafast light pulses. However, the optical analysis is blind to many aspects. Pairing the illumination of the reaction mixture with other online detection schemes proves extremely valuable. Here we present a combination of variable temperature NMR spectroscopy with in-situ illumination and photon-counting to monitor the short-lived intermediates and gain a comprehensive and quantitative picture of the working of a hemithioindigo based molecular motor. Application of the scheme is not limited to the field of molecular machines, we rather think that it will be of great use for any detailed identification and characterization of chemical intermediates in photchemistry, photoredox catalysis, photo-switching, or photo-responsive materials.
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