High Pressure Flow Chemistry Applications

    There are at least four situations where high pump delivery pressures enable more flow chemistry to be explored.

    • High temperatures with volatile solvents
    • Continuous flow polymerization
    • “Flash chemistry”
    • Synthesis of ionic liquids

    The most common of these is to achieve high reaction temperatures while using volatile solvents.

    There are several situations where either volatile solvents, volatile reagents or dissolved gases are involved, and the permissible temperature is effectively limited by the available pressure.   In these instances, a higher pressure capability permits the user to make the most of the available temperature capability.

    For example:

    – Dichloromethane at 250°C requires > 79 bar to prevent it from boiling in the reactor

    – Ethanol at 250°C requires > 66 bar to prevent it from boiling in the reactor

    Vapourtec offer a free chart showing what pressure is required for each solvent to ensure

    that it does not boil at a particular temperature.   It can be found at  the vapour pressure chart page

    Examples of published literature for High Pressure Flow Chemistry Applications

    The Preparation of Ethyl Levulinate Facilitated by Flow Processing: The Catalyzed and Uncatalyzed Esterification of Levulinic Acid

    Meghan P. Negus1, Andrew C. Mansfield2, Nicholas E. Leadbeater1

    • 1 Department of Chemistry, University of Connecticut, 55 North Eagleville Road, Storrs, CT 06269, United States
    • 2 Vapourtec Ltd., Park Farm Business Centre, Bury St. Edmunds IP28 6TS, United Kingdom
    • 3 Department of Community Medicine and Health Care, University of Connecticut Health Center, The Exchange, 263 Farmington Ave, Farmington, CT 06030, United States
    View abstract

    C(sp³)–H functionalisation of N-aryl tetrahydroisoquinolines via an iron-catalysed aerobic nitro-Mannich reaction and continuous flow processing

    Martin Brzozowski, Jose A. Forni, G. Paul Savage and Anastasios Polyzos*

    • CSIRO Manufacturing Flagship, Bayview Avenue, Clayton, Australia
    View abstract

    Glycosylation with N-acetyl glycosamine donors using catalytic iron(III) triflate: from microwave batch chemistry to a scalable continuous-flow process

    Amandine Xolina, Arnaud Stévenina, Mathieu Pucheaultb, Stéphanie Norsikiana, François-Didier Boyer*ac, Jean-Marie Beau*ad

    • aCentre de Recherche de Gif, Institut de Chimie des Substances Naturelles, CNRS, Gif-sur-Yvette, France
    • bInstitut des Sciences Moléculaires, CNRS-Université de Bordeaux, Talence, France
    • cInstitut Jean-Pierre Bourgin, UMR1318 INRA-AgroParisTech, Versailles, France
    • dUniversité Paris-Sud and CNRS, Laboratoire de Synthèse de Biomolécules, Institut de Chimie Moléculaire et des Matériaux, Orsay, France
    View abstract

    Sequential flow process for the controlled polymerisation and thermolysis of RAFT-synthesised polymers

    CH Hornung, A Postma, S Saubern, J Chiefari

    • CSIRO Materials Science and Engineering, Victoria, Australia
    View abstract

    Application Notes regarding High Pressure Flow Chemistry Applications

    Application Note 32: High Pressure and Temperature Process Scale S N Ar Reaction under Solvent Free Conditions using Liquefied Dimethylamine.

    app_note32

    This application note illustrates the use of the Vapourtec R-Series system to run reactions under solvent free (neat) conditions and it’s ability to pump liquefied gases at high temperatures and pressures. This expands on work carried out in Application note 29 (where a game changing throughput of material from a bench top system was demonstrated).

    Read more

    Application Note 23 –  SNAr with dimethylamine

    app_note23

    This example illustrates the use of the Vapourtec R-Series system to react
    dissolved gases under pressure without the use of scale limiting pressure
    reactors (e.g. Parr ‘bombs’). The SnAr displacement of an aryl fluoride with
    dimethylamine is described.

    Read more

    Application Note 19 – Ethoxycarbonylation of Iodotoluene with CO Gas

    app_note19

    This example illustrates the use of the new Vapourtec tube in tube gas reactor combined with the Vapourtec R-Series system to react reagent gases under pressure without the use of scale limiting pressure reactors (e.g. Parr ‘bombs’). Here we describe the catalytic ethoxycarbonylation of iodotoluene with CO gas.

    Read more

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