Desorption electrospray ionization mass spectrometry for monitoring the kinetics of Baeyer-Villiger solid-state organic reactions |
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Authors: | Ying Xie Li-Fang He Shui-Chao Lin Hai-Feng Su Su-Yuan Xie Rong-Bin Huang Lan-Sun Zheng |
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Institution: | aState Key Laboratory for Physical Chemistry of Solid Surfaces, and Department of Chemistry, College of Chemistry and Chemical Engineering, Xiamen University, Xiamen, China |
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Abstract: | Desorption electrospray ionization mass spectrometry (DESI-MS) has been used for monitoring solid-state organic reaction in
ambient air, specifically the Baeyer-Villiger (BV) type reaction involving the oxidation of ketones (benzophenone or deoxybenzoin)
by m-chloroperbenzoic acid (m-CPBA) in solid-state. The DESI mass spectra obtained at regular intervals during the BV reaction
processes are featured, with the amount of ester products increasing as those of ketone reactants decrease. Quantitative analyses
of relative intensities of the product, made to quantify the reaction degree of typical solid-state organic reaction (SSOR),
show a precision with RSDs of around 5% to 12%, though the RSDs for direct analysis of intensities of the reactant or the
product in the solid-state are obviously larger. The kinetics of the Baeyer-Villiger type reactions in solid-state are shown
to be dramatically different, in reaction rate, kinetic curve, as well as concentration dependence, from those of the same
reactions taking place in solution. |
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