A Study of Heterogeneous Catalysis by Nanoparticle‐Embedded Paper‐Spray Ionization Mass Spectrometry

Thin film formats are used to study the Claisen–Schmidt base‐catalyzed condensation of 6‐hydroxy‐1‐indanone with substituted benzaldehydes and to compare the reaction acceleration relative to the bulk. Relative acceleration factors initially exceeded 103 and were on the order of 102 at steady state, although the confined volume reaction was not electrostatically driven. Substituent effects were muted compared to those in the corresponding bulk and microdroplet reactions and it is concluded that the rate‐limiting step at steady state is reagent transport to the interface. Conditions were found that allowed product deposition from the thin film to occur continuously as the reaction mixture was added and as the solvent evaporated. Yields of 74 % and production rates of 98 mg h−1 were reached in a very simple experimental system that could be multiplexed to greater scales.

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Reaction Acceleration in Thin Films with Continuous Product Deposition for Organic Synthesis

Wei

Wleklinski

Ferreira

et al. 2017

Angewandte Chemie

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Accelerating Electrochemical Reactions in a Voltage‐Controlled Interfacial Microreactor

et al. 2020

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Microdroplet chemistry is attracting increasing attention for accelerated reactions at the solution-air interface. We report herein a voltage-controlled interfacial microreactor that enables acceleration of electrochemical reactions which are not observed in bulk or conventional electrochemical cells. The microreactor is formed at the interface of the Taylor cone in an electrospray emitter with a large orifice, thus allowing continuous contact of the electrode and the reactants at/near the interface. As a proof-of-concept, electrooxidative CÀH/NÀH coupling and electrooxidation of benzyl alcohol were shown to be accelerated by more than an order of magnitude as compared to the corresponding bulk reactions. The new electrochemical microreactor has unique features that allow i) voltage-controlled acceleration of electrochemical reactions by voltage-dependent formation of the interfacial microreactor; ii) "reversible" electrochemical derivatization; and iii) in situ mechanistic study and capture of key radical intermediates when coupled with mass spectrometry.

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Reaction Acceleration in Thin Films with Continuous Product Deposition for Organic Synthesis

et al. 2017

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Thin film formats are used to study the Claisen-Schmidt base-catalyzed condensation of 6-hydroxy-1-indanone with substituted benzaldehydes and to compare the reaction acceleration relative to the bulk. Relative acceleration factors initially exceeded 10 and were on the order of 10 at steady state, although the confined volume reaction was not electrostatically driven. Substituent effects were muted compared to those in the corresponding bulk and microdroplet reactions and it is concluded that the rate-limiting step at steady state is reagent transport to the interface. Conditions were found that allowed product deposition from the thin film to occur continuously as the reaction mixture was added and as the solvent evaporated. Yields of 74 % and production rates of 98 mg h were reached in a very simple experimental system that could be multiplexed to greater scales.

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A Study of Heterogeneous Catalysis by Nanoparticle‐Embedded Paper‐Spray Ionization Mass Spectrometry

Cited by 5 publications

References 42 publications

Reaction Acceleration in Thin Films with Continuous Product Deposition for Organic Synthesis

Reaction Acceleration in Thin Films with Continuous Product Deposition for Organic Synthesis

Accelerating Electrochemical Reactions in a Voltage‐Controlled Interfacial Microreactor

Reaction Acceleration in Thin Films with Continuous Product Deposition for Organic Synthesis

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