Magritek

What can you achieve by monitoring your organic syntheses in real-time with NMR-quality information?

Evaluate the application

The Application

Real-time organic synthesis reaction monitoring is an important for maximizing efficiency and reducing waste by measuring the the % reaction completion or the production of impurities or byproducts.

However, spectroscopic methods (ie, FTIR, NIR, UV/VIS) that non-invasively provide continuous data about the reaction can only provide limited information about actual molecular structure, and more rigorous techniques such as Mass Spectrometry or NMR have traditionally been too slow and expensive to be efficacious.

Most organic and medicinal chemists thus use indirect methods to monitor the reaction in real-time and then use NMR as a final step to confirm the structure of their molecule of interest.

We have developed a system that can provide NMR-quality spectral information in real-time, from continuous flow samples:

  • Deliver direct structural information to monitor the synthesis of the molecule of interest.
  • Identify and monitor the creation of unwanted biproducts or impurities at the exact points within the reaction.

We believe that our system may be of use to real-time reaction monitoring for organic and medicinal chemistry applications.

The System

While traditional, high-field NMR systems are not designed to analyze samples in continuous flow due to their needs for cyrogenic conditions and their need to spin the sample to achieve sensitivity, we at Magritek have developed a solid-state NMR system that can provide structural and quantitative measurement of the molecules within the reaction chamber.

The Magritek SpinSolve Benchtop NMR system's design is optimized to achieve exceptionally high-resolution NMR-quality spectra very quickly, without the need for cyrogenics or sample spinning. Further, normal (protonated) solvents can be used, without the need to deuterate the samples.

Further, the SpinSolve system is designed with a completely open bore from top to bottom, allowing for a flow-cell to mount within the magnet, pumping a continuous flow of the sample from your reaction chamber into the magnet for spectral analysis.

Highlights of the SpinSolve NMR System

  • Frequency: 42.5 MHz Proton and 40.1 MHz Fluorine
  • Nuclei: 1H Proton and 19F Fluorine
  • Resolution: 50% linewidth < 1 Hz, 0.55% linewidth < 40 Hz
  • Spinning: Not required for this resolution
  • Sensitivity: > 100:1 for 1% ethylbenzene single scan
  • Lock: Fast automatic lock. Deuterium solvent not required
Example NMR Spectrum (static sample). Ethyl Crotonate 5% in CDCI3 400 mM
Proton Single Scan with resolution enhancement
The flow cell is mounted in the bore of the magnet The sample is pumped from the reaction vessel, into the bottom of the magnet, and is polarised as it travels up towards the RF coil

Sample Data: Hydrogenation of Acetophenone

THE REACTION

The Hydrogenation of Aceteophenone was performed in normal (non-deuterated) solvents, with each reactant at 1% concentration.

STARTING POINT

Close-up of the NMR spectrum at t=0 min, with color-coding of the peaks that identify the reactants and the product. Spectrum is magnified 40X to highlight sensitivity.

END-POINT

Close-up of the NMR spectrum at t=100 min. Again, color-coding of the peaks identify the reactants and the product and relative concentration can be measured. Spectrum is magnified 40X to highlight sensitivity.

CONFIRMATION

The stacked time-series spectra, showing the growth of the peaks associated with the product correlate with Gas Chromatography Results.

Evaluate

Thank you for reviewing the performance data for SpinSolve as an NMR-based tool for real-time reaction monitoring.

We believe this system can provide valuable information and help increase efficiency of organic syntheses. But we want to hear your feedback. We have prepared a short, 6-question survey for you to provide us with your thoughts. Please lick the link to the right and provide us with your reactions to the information we have presented.

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