Nikola Petrović, Graham R. Cumming, Christopher A. Hone, María José Nieves-Remacha, Pablo García-Losada, Óscar de Frutos, C. Oliver Kappe and David Cantillo*,
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引用次数: 0
Abstract
A design of experiments model has been developed to optimize an electrochemical protocol for the decarboxylative N-alkylation of pyrazole in a spinning cylinder electrode reactor. The electrochemical reaction requires the incorporation of molecular sieves as an additive to ensure the absence of moisture and prevent potential electrode corrosion issues. The spinning cylinder electrode reactor proved to be an ideal platform to scale up this transformation, involving a suspension of solid particles, to multigram scales. The reaction model, which showed an excellent fitting with the experimental data, provided insights into the effect of important electrolysis parameters unique to this reactor design, such as the electrode spinning speed, on the reaction conversion and selectivity. Furthermore, the design of experiments also supplied optimal electrolysis parameters for this complex multivariable reaction system, resulting in full conversion of the substrate and excellent selectivity for a 600 mL volume reaction in recirculation flow mode, with a 94% isolated yield for the target N-alkylated product.
期刊介绍:
The journal Organic Process Research & Development serves as a communication tool between industrial chemists and chemists working in universities and research institutes. As such, it reports original work from the broad field of industrial process chemistry but also presents academic results that are relevant, or potentially relevant, to industrial applications. Process chemistry is the science that enables the safe, environmentally benign and ultimately economical manufacturing of organic compounds that are required in larger amounts to help address the needs of society. Consequently, the Journal encompasses every aspect of organic chemistry, including all aspects of catalysis, synthetic methodology development and synthetic strategy exploration, but also includes aspects from analytical and solid-state chemistry and chemical engineering, such as work-up tools,process safety, or flow-chemistry. The goal of development and optimization of chemical reactions and processes is their transfer to a larger scale; original work describing such studies and the actual implementation on scale is highly relevant to the journal. However, studies on new developments from either industry, research institutes or academia that have not yet been demonstrated on scale, but where an industrial utility can be expected and where the study has addressed important prerequisites for a scale-up and has given confidence into the reliability and practicality of the chemistry, also serve the mission of OPR&D as a communication tool between the different contributors to the field.