Das Suchergebnis hat sich seit Ihrer Suchanfrage verändert. Eventuell werden Dokumente in anderer Reihenfolge angezeigt.
  • Treffer 13 von 16
Zurück zur Trefferliste
Zitieren Sie bitte immer diese URN: urn:nbn:de:kobv:b43-435531

“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. 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 algorithm 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. 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 algorithm 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 NMR spectra were recorded with an acquisition time of 5 s, relaxation delay of 15 s. As a proof-of-concept, the thiol-ene coupling between N-boc cysteine methyl ester and allyl alcohol was conducted in non-deuterated solvents while its time-resolved behaviour was characterised with step tracer experiments. Through the application of spectral modeling the signal area for each reactant can be deconvoluted in the online spectra and thus converted to the respective concentrations or molar ratios. The signals which were suitable for direct integration were used herein for comparison purposes of both methods.zeige mehrzeige weniger
Metadaten
Autoren/innen:Simon KernORCiD, Aleksandra Michalik-Onichimowska, Jens Riedel, Ulrich Panne, R. King, Michael MaiwaldORCiD
Persönliche Herausgeber/innen:Christoph Herwig
Dokumenttyp:Beitrag zu einem Tagungsband
Veröffentlichungsform:Graue Literatur
Sprache:Englisch
Titel des übergeordneten Werkes (Englisch):Tagungsband 11. Interdisziplinäres Doktorandenseminar
Jahr der Erstveröffentlichung:2017
Organisationseinheit der BAM:1 Analytische Chemie; Referenzmaterialien
1 Analytische Chemie; Referenzmaterialien / 1.4 Prozessanalytik
Veröffentlichende Institution:Bundesanstalt für Materialforschung und -prüfung (BAM)
Verlag:Gesellschaft Deutscher Chemiker (GDCh)
Verlagsort:Frankfurt a. M.
Erste Seite:33
Letzte Seite:35
DDC-Klassifikation:Naturwissenschaften und Mathematik / Chemie / Analytische Chemie
Freie Schlagwörter:CONSENS; Click Chemistry; Indirect Hard Modeling; Online NMR Spectroscopy; Process Analytical Technology; Process Control; Process Monitoring
Themenfelder/Aktivitätsfelder der BAM:Analytical Sciences
Analytical Sciences / Sensorik
Veranstaltung:11. Interdisziplinäres Doktorandenseminar
Veranstaltungsort:Berlin, Germany
Beginndatum der Veranstaltung:12.03.2017
Enddatum der Veranstaltung:14.03.2017
URN:urn:nbn:de:kobv:b43-435531
Verfügbarkeit des Volltexts:Volltext-PDF für die Öffentlichkeit verfügbar ("Open Access")
Lizenz (Deutsch):License LogoCreative Commons - CC BY-NC-ND - Namensnennung - Nicht kommerziell - Keine Bearbeitungen 4.0 International
Datum der Freischaltung:03.01.2018
Referierte Publikation:Nein
Schriftenreihen ohne Nummerierung:Wissenschaftliche Artikel der BAM