Monitoring Co-Crystal Formation via In Situ Solid-State NMR

Title:
Monitoring Co-Crystal Formation via In Situ Solid-State NMR
Authors:
Mandala, Venkata S.; Loewus, Sarel J.; Mehta, Manish A. ( 0000-0001-7327-0245 )
Abstract:
A detailed understanding of the mechanism of organic cocrystal formation remains elusive. Techniques that interrogate a reacting system in situ are preferred, though experimentally challenging. We report here the results of a solid-state in situ NMR study of the spontaneous formation of a cocrystal between a pharmaceutical mimic (caffeine) and a coformer (malonic acid). Using 13C magic angle spinning NMR, we show that the formation of the cocrystal may be tracked in real time. We find no direct evidence for a short-lived, chemical shift-resolved amorphous solid intermediate. However, changes in the line width and line center of the malonic acid methylene resonance, in the course of the reaction, provide subtle clues to the mode of mass transfer that underlies cocrystal formation.
Citation:
Mandala, Venkata S., Sarel J. Loewus, and Manish A. Mehta. October 2, 2014. “Monitoring Co-Crystal Formation via In Situ Solid-State NMR.” Journal of Physical Chemistry Letters 5(19): 3340-3344.
Publisher:
American Chemical Society
DATE ISSUED:
2014-10-02
Department:
Chemistry and Biochemistry
Type:
Article
PUBLISHED VERSION:
10.1021/jz501699h
PERMANENT LINK:
http://hdl.handle.net/11282/566775

Full metadata record

DC FieldValue Language
dc.contributor.authorMandala, Venkata S.en
dc.contributor.authorLoewus, Sarel J.en
dc.contributor.authorMehta, Manish A.en
dc.date.accessioned2015-08-13T10:33:48Zen
dc.date.available2015-08-13T10:33:48Zen
dc.date.issued2014-10-02en
dc.identifier.citationMandala, Venkata S., Sarel J. Loewus, and Manish A. Mehta. October 2, 2014. “Monitoring Co-Crystal Formation via In Situ Solid-State NMR.” Journal of Physical Chemistry Letters 5(19): 3340-3344.en
dc.identifier.issn1948-7185en
dc.identifier.urihttp://hdl.handle.net/11282/566775en
dc.description.abstractA detailed understanding of the mechanism of organic cocrystal formation remains elusive. Techniques that interrogate a reacting system in situ are preferred, though experimentally challenging. We report here the results of a solid-state in situ NMR study of the spontaneous formation of a cocrystal between a pharmaceutical mimic (caffeine) and a coformer (malonic acid). Using 13C magic angle spinning NMR, we show that the formation of the cocrystal may be tracked in real time. We find no direct evidence for a short-lived, chemical shift-resolved amorphous solid intermediate. However, changes in the line width and line center of the malonic acid methylene resonance, in the course of the reaction, provide subtle clues to the mode of mass transfer that underlies cocrystal formation.en
dc.language.isoen_USen
dc.publisherAmerican Chemical Societyen
dc.identifier.doi10.1021/jz501699hen
dc.subject.departmentChemistry and Biochemistryen
dc.titleMonitoring Co-Crystal Formation via In Situ Solid-State NMRen
dc.typeArticleen
dc.identifier.journalJournal of Physical Chemistry Lettersen
dc.identifier.volume5en
dc.identifier.issue5en
dc.identifier.startpage3340en
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