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“Click” analytics for “click” chemistry – a simple method for calibration-free evaluation of online NMR spectra

  • Currently research in chemical manufacturing moves towards flexible plug-and-play approaches focusing on modular plants, capable of producing small scales on-demand with short down-times between individual campaigns. This approach allows for efficient use of hardware, a faster optimization of the process conditions, and thus, an accelerated introduction of new products to the market [1]. Driven mostly by the search for chemical syntheses under biocompatible conditions, so-called “click” chemistry rapidly became a growing field of research. The resulting simple one-pot reactions are so far only scarcely accompanied by an adequate optimization via comparably straightforward and robust analysis techniques. Here we report on a fast and reliable calibration-free online high field NMR monitoring approach for technical mixtures. It combines a versatile fluidic system, continuous-flow measurement with a time interval of 20 s per spectrum, and a robust, automated algo-rithm to interpret theCurrently research in chemical manufacturing moves towards flexible plug-and-play approaches focusing on modular plants, capable of producing small scales on-demand with short down-times between individual campaigns. This approach allows for efficient use of hardware, a faster optimization of the process conditions, and thus, an accelerated introduction of new products to the market [1]. Driven mostly by the search for chemical syntheses under biocompatible conditions, so-called “click” chemistry rapidly became a growing field of research. The resulting simple one-pot reactions are so far only scarcely accompanied by an adequate optimization via comparably straightforward and robust analysis techniques. Here we report on a fast and reliable calibration-free online high field NMR monitoring approach for technical mixtures. It combines a versatile fluidic system, continuous-flow measurement with a time interval of 20 s per spectrum, and a robust, automated algo-rithm to interpret the obtained data. All spectra were acquired using a 500 MHz NMR spectrometer (Varian) with a dual band flow probe having a 1/16 inch polymer tubing working as a flow cell. Single scan 1H spectra were recorded with an acquisition time of 5 s, relaxation delay of 15 s.zeige mehrzeige weniger

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Metadaten
Autoren/innen:Simon KernORCiD
Koautoren/innen:Aleksandra Michalik-Onichimowska, Jens Riedel, Ulrich Panne, R. King, Michael Maiwald
Dokumenttyp:Posterpräsentation
Veröffentlichungsform:Präsentation
Sprache:Englisch
Jahr der Erstveröffentlichung:2017
Organisationseinheit der BAM:1 Analytische Chemie; Referenzmaterialien
1 Analytische Chemie; Referenzmaterialien / 1.4 Prozessanalytik
DDC-Klassifikation:Naturwissenschaften und Mathematik / Chemie / Analytische Chemie
Freie Schlagwörter:Click chemistry; Data analysis; Online NMR Spectroscopy
Themenfelder/Aktivitätsfelder der BAM:Analytical Sciences
Analytical Sciences / Sensorik
Veranstaltung:11. Doktorandenseminar 2017 des Arbeitskreis Prozessanalytik der GDCh und DECHEMA
Veranstaltungsort:Berlin, Germany
Beginndatum der Veranstaltung:12.03.2017
Enddatum der Veranstaltung:14.03.2017
Verfügbarkeit des Volltexts:Volltext-PDF im Netzwerk der BAM verfügbar ("Closed Access")
Datum der Freischaltung:16.03.2017
Referierte Publikation:Nein