A kind of benzocyclobutene-terminated imide monomer and preparation method and curing method thereof
A technology of benzocyclobutene and imide, which is applied in the field of benzocyclobutene-terminated imide monomer and its preparation, can solve the problems of leaving micropores and reducing the flatness of the film, and achieves high glass Effects of transition temperature, low dielectric constant, and high hydrophobicity
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Embodiment 1
[0028] A method for preparing an imide monomer benzocyclobutene terminated:
[0029] The 13.71g (100mmol) anthranilic acid and 1.63g (10mmol) of trichloroacetic acid was dissolved in 150mL of tetrahydrofuran mixture, to reduce the temperature of the solution to -5 deg.] C, was slowly added dropwise 23.43g (200mmol) and stirring isoamyl nitrite for 2 hours. The reaction generates a large amount of white precipitate which was separated by filtration, followed by addition of 200 mL 1,4-dioxane and 15.92g (300mmol) of acrylonitrile was stirred under nitrogen mixed to form a suspension, warmed to 50 deg.] C for 5 hours. The reaction mixture was filtered, and the solvent was evaporated under reduced pressure to give a brown viscous liquid. Purified by silica gel column chromatography, eluent methylene chloride and petroleum ether selected: a mixed solvent (volume ratio 51) to give a pale yellow oil intermediate compound II, in 50% yield.
[0030]Weighing 6.45g (50mmol) of Intermediate C...
Embodiment 2
[0034] A method for preparing an imide monomer benzocyclobutene terminated:
[0035] Weighed 13.71g (100mmol) anthranilic acid and 1.31g (8mmol) trichloroacetic acid was dissolved in 150mL of methylene chloride mixture, the temperature of the solution was lowered to -5 deg.] C, was slowly added dropwise 35.15g
[0036] (300mmol) isoamyl nitrite and the reaction was stirred for 2.5 hours. The heavy white precipitate was generated by the reaction was separated by filtration, formed into a suspension with stirring 250mL of methylene chloride, was added 21.22g (400mmol) of acrylonitrile to the reaction flask purged with nitrogen and warmed to 50 deg.] C and refluxed for 6 hours. After the reaction liquid was filtered, the solvent was removed by distillation under reduced pressure to give a brown viscous liquid. Purified by silica gel column chromatography, eluent methylene chloride and petroleum ether selected: a mixed solvent (volume ratio 41) to give a pale yellow oil intermediate c...
Embodiment 3
[0041] A method for preparing an imide monomer benzocyclobutene terminated:
[0042] The 13.71g (100mmol) anthranilic acid and 1.96g (12mmol) trichloroacetic acid in 200mL of tetrahydrofuran were mixed and dissolved, the solution temperature was lowered to -5 deg.] C, was slowly added dropwise 17.57g (150mmol) and stirring isoamyl nitrite 1.5 hours. The reaction generates a large amount of white precipitate which was separated by filtration, followed by addition of 300mL 1,2- dichloroethane and 13.27g (250mmol) of acrylonitrile, mixed suspension formed was stirred under nitrogen, heated to reflux for 4 hours 55 ℃ . The reaction mixture was filtered, and the solvent was evaporated under reduced pressure to give a brown viscous liquid. Purified by silica gel column chromatography, eluent methylene chloride and petroleum ether selected: a mixed solvent (volume ratio 31) to give a pale yellow oil intermediate compound II, in 42% yield.
[0043] Weighing 6.45g (50mmol) of Intermediate ...
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