Octaphenyl substituted polyhedral oligomeric silsesquioxane derivative molecular glass and application thereof
A technology of silsesquioxane and molecular glass, which is applied in the field of materials, can solve the problems of poor product repeatability, insufficient purity, and low modification yield, and achieve the effects of high yield, simple synthesis process, and easy separation and purification
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[0077] Example 1
[0078] A preparation method of octaphenyl substituted caged silsesquioxane derivative molecular glass includes the following steps:
[0079] 1) To prepare octa-(7,8-dimethoxybiphenyl) silsesquioxane, the synthetic route reaction formula is as follows:
[0080]
[0081] Under the protection of high-purity nitrogen, add octa(p-iodophenyl substituted) silsesquioxane (20.4g, 10mmol, 1.0eq) and 200ml of redistilled tetrahydrofuran into a 500ml schleck reaction flask, stir to dissolve and add to the reaction flask Add 3,4-dimethoxyphenylboronic acid (18.2g, 100mmol, 10.0eq) and 2M Na 2 CO 3 80ml aqueous solution, and finally add the catalyst Pd(PPh 3 ) 4 (577mg, 0.5mmol, 0.05eq), the reaction solution was heated to 50~70℃ to react for 12h, cooled to room temperature, the reaction solution was extracted with dichloromethane / water, the organic layers were combined, dried over anhydrous sodium sulfate, concentrated under reduced pressure to remove the solvent The residue w...
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[0090] Example 2
[0091] A preparation method of octaphenyl substituted caged silsesquioxane derivative molecular glass includes the following steps:
[0092] 1) Preparation of octa-(7,8,9-trimethoxybiphenyl) silsesquioxane, the synthesis route reaction formula is as follows:
[0093]
[0094] Under the protection of high-purity nitrogen, add octa(p-iodophenyl substituted) silsesquioxane (20.4g, 10mmol, 1.0eq) and 200ml of redistilled tetrahydrofuran into a 500ml schleck reaction flask, stir to dissolve and add to the reaction flask Add 3,4,5-trimethoxyphenylpinacol borane (29.4g, 100mmol, 10.0eq) and 2M Na 2 CO 3 80ml aqueous solution, and finally add the catalyst Pd(PPh 3 ) 4 (577mg, 0.5mmol, 0.05eq), the reaction solution was heated to 50~70℃ to react for 12h, cooled to room temperature, the reaction solution was extracted with dichloromethane / water, the organic layers were combined, dried over anhydrous sodium sulfate, concentrated under reduced pressure to remove the solvent T...
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[0103] Example 3
[0104] Steps 1) and 2) are the same as in Example 1.
[0105] 3) Octa-(7,8-adamantyl diacetate biphenyl) silsesquioxane, the synthetic route reaction formula is as follows:
[0106]
[0107] In the reaction formula, AD means Substituents.
[0108] Add octa-(7,8-dihydroxybiphenyl) silsesquioxane (4.0, 2.1mmol, 1.0eq), tetrabutylammonium bromide (812mg, 2.5mmol, 1.2eq), K 2 CO 3 (4.6g, 33.6mmol, 16.0eq) and N-methylpyrrolidone (NMP, 40ml), stir well at room temperature, slowly add adamantyl chloroacetate (8.15g, 33.6mmol, 16.0eq) to the reaction solution In NMP (20ml) solution, the reaction system was heated to 60°C for 48h. After the reaction was completed, cooled to room temperature, the reaction solution was extracted with ethyl acetate / water, the organic phase was washed once with 3wt% oxalic acid solution and water respectively, the organic layers were combined, dried over anhydrous magnesium sulfate, and the solvent was removed under reduced pressure. The et...
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