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Unveiling Solvent-Mediated Mechanochemical Cocrystallization Pathways by In Situ CLASSIC NMR Spectroscopy.

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|April 27, 2026
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Summary

Solid-state nuclear magnetic resonance (NMR) reveals molecular mechanisms in solvent-assisted mechanochemical synthesis. This technique tracks liquid-assisted grinding reactions, offering insights into polymorphic control and reaction pathways.

Keywords:
NMR spectroscopyliquid-assisted grindingmechanochemistrypharmaceutical cocrystalspolymorphismsolvents effect

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Area of Science:

  • Materials Science
  • Chemical Engineering
  • Pharmaceutical Sciences

Background:

  • Mechanochemical synthesis is a sustainable method for producing pharmaceutical solid forms.
  • The molecular mechanisms of solvent-mediated transformations in mechanochemistry are not well understood.

Purpose of the Study:

  • To develop and apply an in situ solid-state nuclear magnetic resonance (NMR) approach to monitor liquid-assisted grinding reactions.
  • To investigate the role of solvent polarity in mechanochemical cocrystallization.

Main Methods:

  • Utilized a modified CLASSIC NMR protocol under magic-angle spinning conditions.
  • Performed in situ monitoring of theophylline-benzamide and metronidazole-gallic acid cocrystallization with varying solvent polarities.
  • Employed time-resolved in situ X-ray diffraction for complementary analysis.

Main Results:

  • Successfully observed both solid and liquid phases simultaneously during liquid-assisted grinding.
  • Identified transient intermediates, hydrate formation, and solvent-dependent polymorphic outcomes.
  • Demonstrated NMR's capability to capture mechanistic details not accessible by diffraction methods.

Conclusions:

  • Solid-state NMR is a powerful tool for studying solvent effects in mechanochemical synthesis.
  • This approach advances molecular understanding of polymorphic control and reaction pathways.
  • The developed method provides direct mechanistic insights into liquid-assisted grinding reactions.