Rapid chemical reaction monitoring by digital microfluidics-NMR: proof of principle towards an automated synthetic discovery platform

Bing Wu, Sebastian von der Ecken, Ian Swyer, Chunliang Li, Amy Jenne, Franck Vincent, Daniel Schmidig, Till Kuehn, Armin Beck, Falko Busse, Henry Stronks, Ronald Soong, Aaron R. Wheeler (Corresponding author), André Simpson (Corresponding author)

Research output: Contribution to journalArticleAcademicpeer-review

8 Citations (Scopus)

Abstract

Microcoil nuclear magnetic resonance (NMR) has been interfaced with digital microfluidics (DMF) and is applied to monitor organic reactions in organic solvents as a proof of concept. DMF permits droplets to be moved and mixed inside the NMR spectrometer to initiate reactions while using sub-microliter volumes of reagent, opening up the potential to follow the reactions of scarce or expensive reagents. By setting up the spectrometer shims on a reagent droplet, data acquisition can be started immediately upon droplet mixing and is only limited by the rate at which NMR data can be collected, allowing the monitoring of fast reactions. Here we report a cyclohexene carbonate hydrolysis in dimethylformamide and a Knoevenagel condensation in methanol/water. This is to our knowledge the first time rapid organic reactions in organic solvents have been monitored by high field DMF-NMR. The study represents a key first step towards larger DMF-NMR arrays that could in future serve as discovery platforms, where computer controlled DMF automates mixing/titration of chemical libraries and NMR is used to study the structures formed and kinetics in real time.

Original languageEnglish
Pages (from-to)15372-15376
Number of pages5
JournalAngewandte Chemie - International Edition
Volume58
Issue number43
DOIs
Publication statusPublished - 21 Oct 2019

Keywords

  • digital microfluidics
  • hydrolysis
  • NMR spectroscopy
  • rapid reactions
  • reaction monitoring

Fingerprint Dive into the research topics of 'Rapid chemical reaction monitoring by digital microfluidics-NMR: proof of principle towards an automated synthetic discovery platform'. Together they form a unique fingerprint.

  • Cite this

    Wu, B., von der Ecken, S., Swyer, I., Li, C., Jenne, A., Vincent, F., Schmidig, D., Kuehn, T., Beck, A., Busse, F., Stronks, H., Soong, R., Wheeler, A. R., & Simpson, A. (2019). Rapid chemical reaction monitoring by digital microfluidics-NMR: proof of principle towards an automated synthetic discovery platform. Angewandte Chemie - International Edition, 58(43), 15372-15376. https://doi.org/10.1002/anie.201910052