Crosslinking agent and fluorine-containing aromatic compound
一种交联剂、化合物的技术，应用在含氟芳香族化合物领域，能够解决耐蒸气性差等问题，达到改善耐热性和耐蒸气性的效果
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Embodiment 1
[0129] Crosslinker (a) (CF 2 =CF-Ph-CF=CF 2 )Synthesis
[0130] A 500ml two-necked flask equipped with a dry ice condenser and a diaphragm was replaced with Ar, and 2.18g (16mmol) of zinc chloride (ZnCl) dissolved in 30ml of dehydrated tetrahydrofuran (THF) was added. 2 ) THF solution formed. The ZnCl 2 / THF solution was cooled to 15°C, and 2ml (24mmol) of CF was added 3 CH 2 F. After further cooling to 10°C, add 22ml (33mmol) lithium diisopropylamide (about 20% in tetrahydrofuran / ethylbenzene / heptane, about 1.5mol / L) using a syringe (immerse the needle into CF 3 CH 2 F / ZnCl 2 / THF solution, slowly added).
[0131] After stirring at 15° C. for 1 hour, 1.430 g (4.3 mmol) of 1,4-diiodobenzene and 175.3 mg (0.152 mmol) of tetrakis(triphenylphosphine)palladium(0) were added, followed by stirring at room temperature for 24 hours. Thereafter, the solution is concentrated until the solution becomes about 5 to 10 ml, and the target compound is extracted by decantation using ...
Embodiment 2
[0135] Cross-linking agent (h) (CF 2 =CF-Ph-Ph-CF=CF 2 )Synthesis
[0136] A 500ml two-necked flask equipped with a dry ice condenser and a diaphragm was replaced with Ar, and 6.814g (50mmol) of zinc chloride (ZnCl) dissolved in 100ml of dehydrated tetrahydrofuran (THF) was added. 2 ) THF solution formed. The ZnCl 2 / THF solution was cooled to 15°C, and 6ml (72mmol) of CF was added 3 CH 2 F. After further cooling to 10 °C, add 66.7 ml (100 mmol) lithium diisopropylamide (about 20% in tetrahydrofuran / ethylbenzene / heptane, about 1.5 mol / L) using a syringe (immerse the needle into CF 3 CH 2 F / ZnCl 2 / THF solution, added as a solution).
[0137] After stirring at 15°C for 1 hour, 5.684 g (14 mmol) of 4,4'-diiodobenzene and 566.2 mg (0.49 mmol) of tetrakis(triphenylphosphine)palladium(0) were added, followed by stirring at room temperature for 24 hours. Thereafter, the solution was concentrated until the solution became about 20 ml, and the target compound was extracted b...
Embodiment 3
[0141] Crosslinker (c) (CF 2 =CF-Ph-C(CF 3 ) 2 -Ph-CF=CF 2 )Synthesis
[0142] (1)I-Ph-C(CF 3 ) 2 -Synthesis of Ph-I
[0143] Add 2.48g (36mmol) sodium nitrite and 350ml distilled water into a 1000ml eggplant-shaped flask, and cool to 0°C. 15 ml of 6M HCl was added to the solution at a rate of 1.5 ml / min. Further, a solution obtained by dissolving 5.01 g (15 mmol) of 2,2-bis(4-aminophenyl)hexafluoropropane in 30 ml of N,N-dimethylformamide was added at a rate of 2.5 to 3 ml / min, Stir for 30 minutes at 0 to 3°C. Thereafter, slowly add dropwise a solution obtained by dissolving 12.45 g (75 mmol) of potassium iodide in 30 ml of distilled water at 0 to 3°C. If a precipitate forms, add N,N-dimethylformamide (final is about 250ml). After stirring at 0 to 3°C for 1 hour, it was stirred at room temperature for 12 hours.
[0144]The reacted solution was extracted with 500 ml of ether, washed several times with 100 ml of sodium thiosulfate aqueous solution, and further washed...
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