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'Click' functionalization of cryogels conveniently verified and quantified using high-resolution MAS NMR spectroscopy.

Authors
  • Van Camp, Wim
  • Dispinar, Tugba
  • Dervaux, Bart
  • Prez, Filip E Du
  • Martins, José C
  • Fritzinger, Bernd
Type
Published Article
Journal
Macromolecular rapid communications
Publication Date
Aug 03, 2009
Volume
30
Issue
15
Pages
1328–1333
Identifiers
DOI: 10.1002/marc.200900087
PMID: 21638387
Source
Medline
License
Unknown

Abstract

Chemical modification reactions of alkyne containing polyHEMA-based macroporous network structures (cryogels) by Cu(I) catalyzed azide-alkyne 'click' cycloaddition reactions and their monitoring and quantification with high-resolution magic angle spinning (hr-MAS) NMR spectroscopy are reported. Complete conversion is obtained when benzylazide is reacted with the grafted alkyne function, but only partial conversion is observed when using azide-modified poly(ethylene glycol) (PEG-N(3) ). Subsequent addition of benzylazide consumes all remaining alkyne groups. All chemical modifications are easily monitored at each stage using hr-MAS NMR spectroscopy. The alkyne functionality and the resulting triazole ring provide well resolved (1) H resonances to monitor and quantify the progress of such 'click' reactions in general.

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