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@ARTICLE{Hvelmann:834277,
author = {Hövelmann, Claas and Goossen, Sebastian and Allgaier, J.},
title = {{S}cale-{U}p {P}rocedure for the {E}fficient {S}ynthesis of
{H}ighly {P}ure {C}yclic {P}oly(ethylene glycol)},
journal = {Macromolecules},
volume = {50},
number = {11},
issn = {1520-5835},
address = {Washington, DC},
publisher = {Soc.},
reportid = {FZJ-2017-04259},
pages = {4169 - 4179},
year = {2017},
abstract = {Poly(ethylene glycol) (PEG) is ideally suited for the
synthesis of cyclic polymers. The cyclization reaction of
PEG via its tosylate intermediate is well established. We
improved the cyclization reaction and obtained cyclic raw
products in high yields. The quantities of linear precursor
and higher molecular weight condensation byproducts were
low. The latter byproducts can be removed efficiently by
classical fractionation using chloroform/heptane as
solvent/nonsolvent pair. For the removal of linear precursor
a process was developed which comprises the quantitative
oxidation of alcoholic PEG chain ends to carboxyl groups and
their subsequent removal with the help of a basic
ion-exchange resin. The efficient cleaning processes allowed
carrying out the ring closure reaction at relatively high
concentrations and so increasing sample quantities. As a
result, cyclic poly(ethylene glycol) was obtained in high
purity up to a molecular weight of 20 000 g/mol in
quantities of several grams. In order to monitor the
oxidation reaction and to prove the absence of linear
chains, a 1H NMR characterization technique was developed,
which is extremely sensitive up to high molecular weights.},
cin = {ICS-1 / Neutronenstreuung ; JCNS-1},
ddc = {540},
cid = {I:(DE-Juel1)ICS-1-20110106 / I:(DE-Juel1)JCNS-1-20110106},
pnm = {551 - Functional Macromolecules and Complexes (POF3-551) /
6G4 - Jülich Centre for Neutron Research (JCNS) (POF3-623)
/ 6215 - Soft Matter, Health and Life Sciences (POF3-621)},
pid = {G:(DE-HGF)POF3-551 / G:(DE-HGF)POF3-6G4 /
G:(DE-HGF)POF3-6215},
typ = {PUB:(DE-HGF)16},
UT = {WOS:000403530400008},
doi = {10.1021/acs.macromol.7b00361},
url = {https://juser.fz-juelich.de/record/834277},
}