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85033181225
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note
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Synthesis of Polysulfone: In a 300 mL, three-neck flask with a Dean-Stark trap and condenser, bisphenol A (5.36 g, 23.5 mmol) and bis(4-fluorophenyl) sulfone (5.0 g, 19.9 mmol) were dissolved in a solution of N,N-dimethylacetamide (60 mL) and toluene (40mL). Potassium bicarbonate (8.13 g, 58.8 mmol) was then added. The reaction was stirred at 140 °C for 3.5 h. The reaction was then heated to 170 °C for 12 h. Water was collected in the Dean-Stark trap as an azeotropic mixture with toluene. The reaction was that cooled and precipitated into water/methanol (50: 50). The resulting polymer was reprecipitated from THF into water/methanol (2×) and then dried. Mass: 7.5 g. Yield: 79 %.
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note
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Synthesis of Copolymers: To a 10 mL round-bottom flask with magnetic stir bar was added the macroinitiator (1.0 g, 0.25 mmol) dNBipy (202.4 mg, 0.5 mmol), CoBr (36.1 mg, 0.25 mmol), and 1,4-dimethoxybenzene (1.0 g). The flask was sealed with a rubber septum and the contents degassed by applying a vacuum and backfilling with argon (3×). Degassed monomer (Sty, 2.8 mL, 24.8 mmol; BA, 3.6 mL, 24.8 mmol) was then added via syringe. The reaction mixture was heated in a thermostated oil bath (110 °C) while stirring. After 6.75 h, the reaction was cooled and purified by repeated precipitation from THF into MeOH/brine.
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