Polycarbonate with optical activity and preparation method thereof
A polycarbonate and optically active technology, applied in the field of polymer synthesis, can solve problems such as the greenhouse effect, harsh reaction conditions, and single product types, and achieve the effects of broad industrial promotion value, mild reaction conditions, and high optical selectivity
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Embodiment 1
[0018] (1) Add chiral ligand A (Ar=Ph) 0.061 g, 0.1 mmol) and 2 mL toluene into the Schlenk reaction tube, and replace the air in the tube with nitrogen. Slowly add ZnEt dropwise at 0°C (ice-water bath) under nitrogen protection 2 (organometallic; 0.2 mL, 1.0 M, 0.2 mmol), and stirred at room temperature for 30 min. Then add absolute ethanol (0.04 mL, 1 M, 0.04 mmol), continue stirring at room temperature for 15 min, then add 2 mmol of 7-oxobicyclo[4.1.0]-3-heptene (1a), and bubble with carbon dioxide , stirred at 30 °C for 36 h.
[0019] Add 40 mL of dichloromethane to the reaction system for dilution, the organic phase was washed with 1 M hydrochloric acid (3×20 mL) and saturated sodium chloride solution (2×20 mL), and the organic phase was dried over anhydrous magnesium sulfate. Concentrate under reduced pressure to about 3 mL, add 40 mL of methanol to precipitate the polymer, filter, wash with methanol, and dry the product to constant weight to obtain a white solid poly ...
Embodiment 2
[0023] (1) Add chiral ligand A (Ar=Ph) 0.061 g, 0.1 mmol) and 2 mL toluene into the Schlenk reaction tube, and replace the air in the tube with nitrogen. Slowly add ZnEt dropwise at 0°C (ice-water bath) under nitrogen protection 2 (organometallic; 0.2 mL, 1.0 M, 0.2 mmol), and stirred at room temperature for 30 min. Then absolute ethanol (0.04 mL, 1 M, 0.04 mmol) was added, stirring was continued at room temperature for 15 min, then 2 mmol of cyclopentene oxide (1b) was added, carbon dioxide was bubbled, and the reaction was stirred at 30 °C for 36 h.
[0024] Add 40 mL of dichloromethane to the reaction system for dilution, the organic phase was washed with 1 M hydrochloric acid (3×20 mL) and saturated sodium chloride solution (2×20 mL), and the organic phase was dried over anhydrous magnesium sulfate. Concentrate under reduced pressure to about 3 mL, add 40 mL of methanol to precipitate the polymer, filter, wash with methanol, and dry the product to constant weight to obtai...
Embodiment 3
[0028] (1) Add chiral ligand A (Ar=Ph) 0.061 g, 0.1 mmol) and 2 mL toluene into the Schlenk reaction tube, and replace the air in the tube with nitrogen. Slowly add ZnEt dropwise at 0°C (ice-water bath) under nitrogen protection 2 (organometallic; 0.2 mL, 1.0 M, 0.2 mmol), and stirred at room temperature for 30 min. Then add absolute ethanol (0.04 mL, 1 M, 0.04 mmol), continue stirring at room temperature for 15 min, and then add 2 mmol of 4,4-dimethyl-3,5,8-trioxobicyclo[5.1.0 ] octane (1c), carbon dioxide bubbles, 30 ℃ stirring reaction for 36 h.
[0029] Add 40 mL of dichloromethane to the reaction system for dilution, the organic phase was washed with 1 M hydrochloric acid (3×20 mL) and saturated sodium chloride solution (2×20 mL), and the organic phase was dried over anhydrous magnesium sulfate. Concentrate under reduced pressure to about 3 mL, add 40 mL of methanol to precipitate the polymer, filter, wash with methanol, and dry the product to constant weight. 0.321 g ...
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