Poly(arylene ether sulfone)
A technology of aryl ether sulfone and dihaloaryl, applied in the field of polyarylene ether sulfone, which can solve the problems of extraction, lack of l-idose, etc.
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example 18
[0199] Example 18: 4,4'-dichlorodiphenyl sulfone (DCDPS) as dihalogen (B Cl B Cl ) of the "Halex" reaction provides a mixture of Halex products
[0200] A 50 ml round bottom flask was charged with 1.0 g (3.484 mmol) DCDPS and 2.1 g (13.94 mmol) CsF and 3.54 g sulfolane and heated to 210°C using an oil bath. The Hallex reaction was carried out at this temperature for 24 hours. After completion of the reaction, a small sample of the reaction mixture was diluted with dichloromethane and treated with activated charcoal to remove color bodies and the dichloromethane solution was removed by rotary evaporator. The residual product was analyzed by GC. GC analysis of the isolated product showed 90.8% DFDPS, 6.7% 4-chloro-4'-fluoro-diphenylsulfone and 2.5% DCDPS starting material.
example 19
[0201] Example 19: 4,4'-dichlorodiphenyl sulfone (DCDPS) as dihalogen (B Cl B Cl ) of the "Halex" reaction provides a mixture of Halex products
[0202]A 50 ml round bottom flask was charged with 2.0 g (6.96 mmol) DCDPS and 2.1 g (13.94 mmol) CsF and 5.0 g sulfolane and heated to 210°C using an oil bath. The Hallex reaction was carried out at this temperature for 24 hours. After completion of the reaction, a small sample of the reaction mixture was diluted with dichloromethane and treated with activated charcoal to remove color bodies and the dichloromethane solution was removed by rotary evaporator. The residual product was analyzed by GC. GC analysis of the isolated product showed 90.5% DFDPS and 9.5% 4-chloro-4'-fluoro-diphenylsulfone.
example 20
[0203] Example 20: 4,4'-dichlorodiphenyl sulfone (DCDPS) as dihalogen (B Cl B Cl ) "Halex" reaction in the presence of PTC provides a mixture of Hallex products
[0204] A 1 L three-neck round bottom flask equipped with a mechanical stirrer with nitrogen inlet and outlet was charged with 253.33 g (0.8823 mol) of DCDPS, 205.0 g (3.529 mol) of anhydrous KF, 10.86 g (4.411 mmol) of 18-crown -6, and 406 g of sulfolane. The mixture was gradually heated to 210° C. in an oil bath and the reaction was carried out at this temperature for 20 hours. After completion of the reaction, the reaction mixture was filtered through a high pressure filter to remove excess salt and dichloromethane was added to the filtered solution. Then deionized water was added to dichloromethane and the organic layer was separated. Then, the organic layer was washed again with deionized water to remove residual sulfolane. Add some activated charcoal to the collected organic layer to remove the color and ad...
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