Packed‐Bed Reactors for Continuous‐Flow CN Cross‐Coupling

Naber, John R.; Buchwald, Stephen L.

doi:10.1002/anie.201004425

Cited by 108 publications

(75 citation statements)

References 58 publications

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“…However, such reactors typically give rise to poorly defined interfacial areas and the yield is strongly dependent on the stirring efficiency. Beside this, packed-bed microreactors can further improve the mass transfer between two immiscible liquid phases efficiently [28][29][30][31][32][33]. 1000 m 2 m -3 are feasible in stirred reactors [22].…”

Section: Introductionmentioning

confidence: 99%

Packed‐Bed Microreactor for Continuous‐Flow Adipic Acid Synthesis from Cyclohexene and Hydrogen Peroxide

et al. 2013

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The synthesis of adipic acid by means of a direct oxidation of cyclohexene by hydrogen peroxide was carried out in a continuous-flow packed-bed microreactor. The reaction uses Na 2 WO 4 ·2H 2 O as a catalyst and [CH 3 (n-C 8 H 17 ) 3 N]HSO 4 as a phase transfer catalyst without additional solvent. A parametric process optimization, such as glass beads size, residence time, concentration of hydrogen peroxide, addition of acid, reaction temperature, and molar ratios of reactants and catalysts, was performed. It is demonstrated that smaller glass beads result in a better yield of adipic acid and that the addition of acid plays an important role in the oxidation of cyclohexene to adipic acid. Based on the concept of Novel Process Windows, the influence of elevated temperatures is investigated.

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Section: Introductionmentioning

confidence: 99%

Packed‐Bed Microreactor for Continuous‐Flow Adipic Acid Synthesis from Cyclohexene and Hydrogen Peroxide

et al. 2013

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“…Examples of this strategy are biphasic reaction conditions in which water is added as a second phase to dissolve inorganic salts. 50,53 Insoluble materials can be transported through the microreactor channels as a slurry. 158 However, this strategy works best when a segmented flow regime is used where intensified mixing patterns in the liquid slugs keep the particles in suspension and avoids interaction with the reactor walls.…”

Section: Solids Handling In Flowmentioning

confidence: 99%

Beyond Organometallic Flow Chemistry: The Principles Behind the Use of Continuous-Flow Reactors for Synthesis

Noël

Hessel

2015

Topics in Organometallic Chemistry

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Flow chemistry is typically used to enable challenging reactions which are difficult to carry out in conventional batch equipment. Consequently, the use of continuous-flow reactors for applications in organometallic and organic chemistry has witnessed a spectacular increase in interest from the chemistry community in the last decade. However, flow chemistry is more than just pumping reagents through a capillary and the engineering behind the observed phenomena can help to exploit the technology's full potential. Here, we give an overview of the most important engineering aspects associated with flow chemistry. This includes a discussion of mass-, heat-, and photon-transport phenomena which are relevant to carry out chemical reactions in a microreactor. Next, determination of intrinsic kinetics, automation of chemical processes, solids handling and multistep reaction sequences in flow are discussed. Safety is one of the main drivers to implement continuous-flow microreactor technology in an existing process and a brief overview is given here as well. Finally, the scale-up potential of microreactor technology is reviewed.

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“…To obtain the reaction profiles in a flow setting, we assembled a continuous‐flow setup by using syringe pumps, perfluoroalkoxyalkane (PFA) tubing, T‐ and cross‐junctions, and a packed‐bed reactor (see the Supporting Information). Tubular reactors filled with stainless steel spheres (diameter: 60–120 μm) have previously been used in continuous‐flow reactions to efficiently enhance biphasic mass‐ and heat‐transfer processes 13b,e,g. Initially, a stock solution of allylpalladium chloride dimer in 1,4‐dioxane was used as one of the streams and was pumped into the reaction.…”

Section: Optimizations Under Batch Conditions[a]mentioning

confidence: 99%

A Microfluidic System for the Continuous Recycling of Unmodified Homogeneous Palladium Catalysts through Liquid/Liquid Phase Separation

Li¹,

Moore²,

Jensen³

2013

ChemCatChem

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Packed‐Bed Reactors for Continuous‐Flow CN Cross‐Coupling

Cited by 108 publications

References 58 publications

Packed‐Bed Microreactor for Continuous‐Flow Adipic Acid Synthesis from Cyclohexene and Hydrogen Peroxide

Packed‐Bed Microreactor for Continuous‐Flow Adipic Acid Synthesis from Cyclohexene and Hydrogen Peroxide

Beyond Organometallic Flow Chemistry: The Principles Behind the Use of Continuous-Flow Reactors for Synthesis

A Microfluidic System for the Continuous Recycling of Unmodified Homogeneous Palladium Catalysts through Liquid/Liquid Phase Separation

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