Polycyclic carbonate compound and preparation method thereof
A technology for cyclic carbonates and compounds, applied in the field of polycyclic carbonates and their preparation, can solve the problems of less reports of alkyne and carbon dioxide copolymerization, and achieve unique post-modification performance, excellent processability, and cost. low effect
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Embodiment 1
[0048] A kind of polycyclic carbonate compound P1a / 2a / CO of the present embodiment 2 , its structural formula is as follows:
[0049]
[0050] The above-mentioned polycyclic carbonate compounds are prepared by the polymerization reaction of difunctional acetylenic alcohol monomers, carbon dioxide and dihalide monomers, and the reaction equation is as follows:
[0051]
[0052] Wherein, the synthetic route of monomer 1a is as follows:
[0053]
[0054] Concrete synthetic steps are as follows:
[0055] Add 5 (2.61g, 5mmol), 6 (1.21mL, 12.5mmol), Pd(PPh 3 ) 2 Cl 2 (176mg, 0.25mmol), CuI (48mg, 0.25mmol), vacuum three times for nitrogen, then added tetrahydrofuran (THF) 60 ml, added triethylamine (Et 3 N) 30 milliliters, heated and refluxed for 12 hours, then filtered the reaction solution to remove the precipitate, repeatedly washed the precipitate three times with dichloromethane (DCM) in the process, collected and concentrated the filtered solution, separated and ...
Embodiment 2
[0068] A kind of polycyclic carbonate compound P1a / 2b / CO of the present embodiment 2 , its structural formula is as follows:
[0069]
[0070] The above-mentioned polycyclic carbonate compounds are prepared by the polymerization reaction of difunctional acetylenic alcohol monomers, carbon dioxide and dihalide monomers, and the reaction equation is as follows:
[0071]
[0072] Wherein, the synthesis method of monomer 1a is shown in Example 1.
[0073] The specific preparation steps of the polycyclic carbonate compound described in the present embodiment are as follows:
[0074] In a dry Schlenk tube add 1a (43.5 mg, 0.1 mmol), 2b (42.2 mg, 0.1 mmol), Pd(OAc) 2 (2.3mg, 0.01mmol), LiO t Bu (48.0mg, 0.6mmol), vacuumize for 0.5 hours, tie a balloon filled with carbon dioxide on the tube, add N,N-dimethylformamide (DMF) 1mL, react at 80°C for 2.5 hours, then cool to room temperature, After the reaction, the solution was first diluted with 4 mL of DCM, then passed through ...
Embodiment 3
[0083] A kind of polycyclic carbonate compound P1b / 2a / CO of the present embodiment 2 , its structural formula is as follows:
[0084]
[0085] The above-mentioned polycyclic carbonate compounds are prepared by the polymerization reaction of difunctional acetylenic alcohol monomers, carbon dioxide and dihalide monomers, and the reaction equation is as follows:
[0086]
[0087] Wherein, the synthesis method of monomer 1b can refer to Example 1.
[0088] The specific preparation steps of the polycyclic carbonate compound described in the present embodiment are as follows:
[0089] In a dry Schlenk tube was added 1b (57.7 mg, 0.1 mmol), 2a (33.0 mg, 0.1 mmol), Pd(OAc) 2 (2.3mg, 0.01mmol), LiO t Bu (48.0mg, 0.6mmol), vacuumize for 0.5 hours, tie a balloon filled with carbon dioxide on the tube, add N,N-dimethylformamide (DMF) 1mL, react at 80°C for 4 hours, then cool to room temperature, After the reaction, the solution was first diluted with 4 mL of DCM, then passed thr...
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