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3 solution referenced to external TMS.
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note
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The polymerization of the purified dichlorosilanes was performed according to the conventional Wurtz-type condensation as follows. The synthesis of 1 is representative. To a mixture of 16 mL of dry toluene, 1.3 g (0.06 mol) of sodium dispersion, and surface-activated by diglyme (10 μL), 4.0 g (0.014 mol) of methyl-m-(S)-2-methylbutoxyphenyldichlorosilane was added dropwise in an argon atmosphere. The mixture was stirred slowly at 110 °C, monitoring the molecular weight periodically. After 2 h, 0.1 equiv of trimethylchlorosilane was added as terminator, and stirring continued for a further 30 min and then cooled to room temperature. The mixture was hydrolyzed with ethanol and water. The organic layer was separated and washed with water. After the solvent was removed, the remaining crude polymer was reprecipitated from toluene-ethanol solution. The high molecular weight fraction was obtained as a white powder, separated by centrifugation, and vacuum-dried in an oven at 90 °C for 5 h. The yields and some properties of polysilanes 1-4 obtained in this work are summarized in Table 1.
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