Benzocyclobutene-substituted triethylenecyclohexane compound and preparation method thereof, organic dielectric material and preparation method thereof
A technology of benzocyclobutene and bromobenzocyclobutene, which is applied in the field of organic dielectric materials and its preparation, can solve problems such as difficulty in obtaining low dielectric properties, decreased dielectric properties, and difficulties in mass production, and achieves a convenient large-scale Large-scale production, lower dielectric constant, and low-cost effects
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Embodiment 1
[0047]In a flask, 91.5 mg of 0.5 mmol 4-bromobenzocyclobutene (BBCB) and 81 mg of 0.5 mmol 1,2,4-trivinylcyclohexane (TVCH) were weighed. 14 mg of 0.029 mmol tris(o-methylphenyl)phosphine, 7 mg of palladium acetate 0.018 mmol, 0.3 ml of triethylamine, 1 ml of acetonitrile, and stirred at 85°C for 24 hours in an argon atmosphere. Cool and spin dry the solvent. Quickly pass through the column with neutral alumina, spin dry the solvent to obtain a yellow-green solid, recrystallize from methanol, and vacuum dry to obtain 47 mg of a colorless viscous liquid with a yield of 35.6%. reaction process such as figure 1 shown.
[0048] The nuclear magnetic spectrum of the benzocyclobutene-substituted triethylenecyclohexane compound prepared in this example is as follows: figure 2 shown.
[0049] The benzocyclobutene-substituted triethylenecyclohexane compound prepared in this example is thermally cured to prepare a benzocyclobutene derivative thermally curable resin, that is, an orga...
Embodiment 2
[0055] In a flask, 183 mg of 1 mmol of 4-bromobenzocyclobutene (BBCB) and 81 mg of 0.5 mmol of 1,2,4-trivinylcyclohexane (TVCH) were weighed. 14 mg of 0.029 mmol tris(o-methylphenyl)phosphine, 7 mg of palladium acetate 0.018 mmol, 0.3 ml of triethylamine, 1 ml of acetonitrile, and stirred at 85°C for 24 hours in an argon atmosphere. Cool and spin dry the solvent. Quickly pass through the column with neutral alumina, spin dry the solvent to obtain a yellow-green solid, recrystallize from methanol, and vacuum dry to obtain 73 mg of a colorless colloidal solid with a yield of 40%. reaction process such as Figure 5 shown.
[0056] The nuclear magnetic spectrum of the benzocyclobutene-substituted triethylenecyclohexane compound prepared in this example is as follows: Image 6 shown.
[0057] The benzocyclobutene-substituted triethylenecyclohexane compound prepared in this example is thermally cured to prepare a benzocyclobutene derivative thermally curable resin, that is, an o...
Embodiment 3
[0063] In a flask, 302 mg of 1.65 mmol of 4-bromobenzocyclobutene (BBCB) and 81 mg of 0.5 mmol of 1,2,4-trivinylcyclohexane (TVCH) were weighed. 14 mg of 0.029 mmol tris(o-methylphenyl)phosphine, 7 mg of palladium acetate 0.018 mmol, 0.3 ml of triethylamine, 1 ml of acetonitrile, and stirred at 85°C for 24 hours in an argon atmosphere. Cool and spin dry the solvent. Quickly pass through the column with neutral alumina, spin dry the solvent to obtain a yellow-green solid, recrystallize from methanol, and vacuum dry to obtain 168 mg of a yellow-green solid with a yield of 71.8%. reaction process such as Figure 9 shown.
[0064] The nuclear magnetic spectrum of the benzocyclobutene-substituted triethylenecyclohexane compound prepared in this example is as follows: Figure 10 shown.
[0065] The benzocyclobutene-substituted triethylenecyclohexane compound prepared in this example is thermally cured to prepare a benzocyclobutene derivative thermally curable resin, that is, an ...
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