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      Extrusion – back to the future: Using an established technique to reform automated chemical synthesis

      review-article
      1 ,
      Beilstein Journal of Organic Chemistry
      Beilstein-Institut
      continuous, extrusion, industry, organic, synthesis

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          Summary

          Herein, the benefits which extrusion can provide for the automated continuous synthesis of organic compounds are highlighted. Extrusion is a well-established technique that has a vital role in the manufacturing processes of polymers, pharmaceuticals and food products. Furthermore, this technique has recently been applied to the solvent-free continuous synthesis of co-crystals and coordination compounds including metal-organic frameworks (MOFs). To date, a vast amount of research has already been conducted into reactive extrusion (REX), particularly in the polymer industry, which in many cases has involved organic transformations, however, it has not received significant recognition for this. This review highlights these transformations and discusses how this previous research can be applied to the future of organic compound manufacture.

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          Most cited references39

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          Industrial applications of metal-organic frameworks.

          New materials are prerequisite for major breakthrough applications influencing our daily life, and therefore are pivotal for the chemical industry. Metal-organic frameworks (MOFs) constitute an emerging class of materials useful in gas storage, gas purification and separation applications as well as heterogeneous catalysis. They not only offer higher surface areas and the potential for enhanced activity than currently used materials like base metal oxides, but also provide shape/size selectivity which is important both for separations and catalysis. In this critical review an overview of the potential applications of MOFs in the chemical industry is presented. Furthermore, the synthesis and characterization of the materials are briefly discussed from the industrial perspective (88 references).
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            Natural deep eutectic solvents as new potential media for green technology.

            Developing new green solvents is one of the key subjects in Green Chemistry. Ionic liquids (ILs) and deep eutectic solvents, thus, have been paid great attention to replace current harsh organic solvents and have been applied to many chemical processing such as extraction and synthesis. However, current ionic liquids and deep eutectic solvents have still limitations to be applied to a real chemical industry due to toxicity against human and environment and high cost of ILs and solid state of most deep eutectic solvents at room temperature. Recently we discovered that many plant abundant primary metabolites changed their state from solid to liquid when they were mixed in proper ratio. This finding made us hypothesize that natural deep eutectic solvents (NADES) play a role as alternative media to water in living organisms and tested a wide range of natural products, which resulted in discovery of over 100 NADES from nature. In order to prove deep eutectic feature the interaction between the molecules was investigated by nuclear magnetic resonance spectroscopy. All the tested NADES show clear hydrogen bonding between components. As next step physical properties of NADES such as water activity, density, viscosity, polarity and thermal properties were measured as well as the effect of water on the physical properties. In the last stage the novel NADES were applied to the solubilization of wide range of biomolecules such as non-water soluble bioactive natural products, gluten, starch, and DNA. In most cases the solubility of the biomolecules evaluated in this study was greatly higher than water. Based on the results the novel NADES may be expected as potential green solvents at room temperature in diverse fields of chemistry. Copyright © 2012 Elsevier B.V. All rights reserved.
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              Synthesis by extrusion: continuous, large-scale preparation of MOFs using little or no solvent † †Electronic supplementary information (ESI) available. See DOI: 10.1039/c4sc03217a Click here for additional data file.

              Continuous flow mechanochemical and melt-phase synthesis at kg h–1 rates from solid reagents and either no solvent, or only minimal solvent, is reported.
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                Author and article information

                Contributors
                Role: Guest Editor
                Journal
                Beilstein J Org Chem
                Beilstein J Org Chem
                Beilstein Journal of Organic Chemistry
                Beilstein-Institut (Trakehner Str. 7-9, 60487 Frankfurt am Main, Germany )
                1860-5397
                2017
                11 January 2017
                : 13
                : 65-75
                Affiliations
                [1 ]Queen’s University Belfast, School of Chemistry and Chemical Engineering, David Keir Building, 39–123 Stranmillis Road, Belfast, BT9 5AG, Northern Ireland, UK
                Article
                10.3762/bjoc.13.9
                5238592
                2eccacf8-c3a2-4052-b894-aa27e72d5372
                Copyright © 2017, Crawford; licensee Beilstein-Institut.

                This is an Open Access article under the terms of the Creative Commons Attribution License ( http://creativecommons.org/licenses/by/4.0), which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited.

                The license is subject to the Beilstein Journal of Organic Chemistry terms and conditions: ( http://www.beilstein-journals.org/bjoc)

                History
                : 15 October 2016
                : 29 December 2016
                Categories
                Review
                Chemistry
                Organic Chemistry

                Organic & Biomolecular chemistry
                continuous,extrusion,industry,organic,synthesis
                Organic & Biomolecular chemistry
                continuous, extrusion, industry, organic, synthesis

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