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The separated MEK-insoluble fractions of the polymers obtained under conditions producing a large amount of highmolecular weight parts (e.g., without additives, in the presence of DTBP, etc.) often became hard to be dissolved in various solvents once they were completely dried. Thus, for such polymers, the gelled portions obtained after centrifuging the mixtures in MEK were diluted with dichloromethane to yield homogeneous solutions. The solutions were left in air or under reduced pressure to gradually evaporate the solvents, dichloromethane and the residual MEK. Then, carbon tetrachloride was added and evaporated for several times to remove MEK as much as possible. Finally, the concentrated but still transparent solutions were diluted with solvents for the NMR and GPC measurements
-
The separated MEK-insoluble fractions of the polymers obtained under conditions producing a large amount of highmolecular weight parts (e.g., without additives, in the presence of DTBP, etc.) often became hard to be dissolved in various solvents once they were completely dried. Thus, for such polymers, the gelled portions obtained after centrifuging the mixtures in MEK were diluted with dichloromethane to yield homogeneous solutions. The solutions were left in air or under reduced pressure to gradually evaporate the solvents, dichloromethane and the residual MEK. Then, carbon tetrachloride was added and evaporated for several times to remove MEK as much as possible. Finally, the concentrated but still transparent solutions were diluted with solvents for the NMR and GPC measurements.
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w values to those obtained without additives. The MEK-insoluble fraction was the largest (19 wt %; 20 mM DTBP) among all the polymers obtained in the present study
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w values to those obtained without additives. The MEK-insoluble fraction was the largest (19 wt %; 20 mM DTBP) among all the polymers obtained in the present study.
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note
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4 under various conditions have a broad peak around the region. The peak seems to mainly contain the latter acetal, although the former derived from MeOH used as a quencher may be present in some degree. However, the similarity in the shapes of the acetal peaks among the polymers obtained without alcohols and with MeOH or iPrOH indicates the less efficient participation of the two alcohols in the polymerizations.
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