Hyperbranched polymer containing crown ether and synthesis process therefor
A hyperbranched polymer and polymer technology, applied in the field of hyperbranched polymerization, can solve problems such as polymer methods not involving hyperbranching, and achieve high ion selectivity
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Embodiment 1
[0043] Embodiment 1, obtain hyperbranched polymer reaction process by 4,4'(5')-dibromomethyl dibenzo-18-crown-6(1) and 1,3,5-benzenetriol as follows: 4,4'(5')-Dibromomethyldibenzo-18-crown-6 (0.3 g, 0.55 mmol) was dissolved in 7.5 mL of dried, redistilled N,N-dimethylformamide ( DMF), stirred and dissolved under the protection of nitrogen, added 1,3,5-benzenetriol (58mg, 0.46mmol), added lithium hydroxide (67mg, 2.79mmol) under stirring, stirred at room temperature (RT=20°C) , point the TLC plate, the reaction is complete after 20h, and then continue to react for 5h. After the reaction, the reaction solution was concentrated to 2mL under reduced pressure, and 30mL of water was added to obtain a clear transparent brown solution, which was acidified with 5% dilute hydrochloric acid to pH=4-5, and a precipitate appeared. After standing overnight, it was filtered to obtain 335mg of the initial product , the initial product was dissolved in 5mL of DMF, precipitated with 30mL of di...
Embodiment 2
[0044]Embodiment 2, obtain the hyperbranched polymer reaction process by 4,4'(5')-dichloromethyl dibenzo-18-crown-6(2) and 1,3,5-benzenetriol as follows: 4,4'(5')-Dichloromethyldibenzo-18-crown-6 (0.25 g, 0.55 mmol) was dissolved in 5.5 mL of dried, redistilled N,N-dimethylformamide (DMF ), stirring and dissolving under the protection of nitrogen, adding (58mg, 0.46mmol) 1,3,5-benzenetriol, adding sodium hydroxide (111mg, 2.79mmol) under stirring, stirring the reaction at 50°C, pointing to a TLC plate, After 40h, the reaction was complete, and the reaction was continued for 8h. After the reaction, the reaction solution was concentrated to 2 mL under reduced pressure, and 30 mL of water was added to obtain a clear transparent brown solution, which was acidified with 5% dilute hydrochloric acid to pH=4-5, and a precipitate appeared, and was filtered after standing overnight to obtain 326 mg of the initial product , the initial product was dissolved in 5mL of DMF, precipitated w...
Embodiment 3
[0045] Example 3. In this example, hyperbranched polymer reaction is obtained by reacting 4,4'(5')-diaminodibenzo-18-crown-6(5) with 1,3,5-trimesic acid The procedure was as follows: 4,4'-diaminodibenzo-18-crown-6 (1.0 g, 2.56 mmol), 1,3,5-trimesic acid (488 mg, 2.23 mmol), 1.90 mL of pyridine and 40 mL Put N-methylpyrrolidone (NMP) into a 100mL Schlenk tube, stir to dissolve it under nitrogen protection, then add triphenyl phosphite (2mL, 7.68mmol), stir the reaction solution and heat up to 80°C for 3h, Then the reaction solution was poured into 120mL of methanol containing 2.5mL of concentrated hydrochloric acid, the product was precipitated in methanol, filtered to obtain 1.87 grams of crude product, the crude product was dissolved in 40mL of N-methylpyrrolidone (NMP), and precipitated with 150mL of methanol , After suction filtration, the product was washed with hot methanol and dried in vacuo to obtain 1.52 g of brown powdery solid. Yield = 76.61%, Mn = 18320, Mw = 28580...
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