 ISSN 0235-7216 ISSN 2424-4538 (online) |
2008 m. Nr. 2 Iodination ofpoly(ethylene glycol) by a mixture of triphenyl phosphite and iodomethane
Iodination of poly(ethylene glycol) (PEG) with the molecular weight 2000 and its monomethyl ether (MPEG) by the iodinating mixture of triphenyl phosphite and iodomethane was studied in detail. The structure of the synthesized PEG (MPEG) iodides was confirmed by elemental analysis, FT-IR and 1H NMR spectroscopy. The degree of iodination (DI) of PEG (MPEG) was determined by two independent methods based on argentometric titration and 1H NMR spectra. Argentometric titration the (Mohr method) was found to be limited by the incomplete hydrolysis of PEG (MPEG) iodides, while the analysis based on 1H NMR spectroscopy became accurate at a high DI only. The highest DI of PEG (MPEG) was reached carrying out the reaction of iodination in a hermetic reactor at 120 °C for 5 hours and using a double-fold excess of the iodinating mixture. The synthesized PEG (MPEG) iodides with DI 90–95 mol% could be useful for “grafting to” or even for polycondensation with diamines. Keywords: poly(ethylene glycol), iodination, PEG, Mohr method, PEGylation |
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