期刊
MACROMOLECULAR RAPID COMMUNICATIONS
卷 30, 期 15, 页码 1328-1333出版社
WILEY-V C H VERLAG GMBH
DOI: 10.1002/marc.200900087
关键词
'click' chemistry; cryogel; functionalization; high-resolution MAS NMR spectroscopy; macroporous networks
资金
- FWO
- ESF-program STIPOMAT
- Belgian Program on Interuniversity Attraction Poles initiated by the Belgian State
- Prime Minister's office (Program P6/27)
- Fund for Scientific Research - Flanders (FWO-Vlaanderen) [G.0365.03, G.0064.07]
- Ghent University the Free University of Brussels (VUB)
- University of Antwerp via the 'Zware Apparatuur' Incentive of the Flemish Government
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 H-1 resonances to monitor and quantify the progress of such 'click' reactions in general.
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