Benzocyclobutene substituted triethylene cyclohexane 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 their preparation, can solve the problems of difficulty in obtaining low dielectric, decreased dielectric properties, difficulty in mass production, etc. The effect of mass production, lower dielectric constant, and low price
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Embodiment 1
[0047] In a flask, 0.5 mmol 4-bromobenzocyclobutene (BBCB) 91.5 mg, 0.5 mmol 1,2,4-trivinylcyclohexane (TVCH) 81 mg were weighed. 0.029 mmol tris(o-methylphenyl)phosphine 14 mg, 0.018 mmol palladium acetate 7 mg, 0.3 ml triethylamine, 1 ml acetonitrile, stirred at 85 degrees in an argon atmosphere for 24 hours. Cool, spin-dry solvent. Neutral alumina was used to quickly pass the column, the solvent was whizzed dry to obtain a yellow-green solid, methanol was recrystallized, and 47 mg of colorless viscous liquid was obtained by vacuum drying, with a yield of 35.6%. Reaction processes such as Figure 1 as shown.
[0048] The nuclear magnetic profile of benzocyclobutene-substituted triethylenecyclohexane compounds prepared in the present embodiment, as shown in Figure 2 as shown.
[0049] The benzocyclobutene substituted triethylenecyclohexane compound prepared from the present embodiment is thermally cured, and the benzocyclobutene derivative is prepared to be heat-cured resin, i.e....
Embodiment 2
[0055] Weigh 1 mmol 4-bromobenzocyclobutene (BBCB) 183 mg and 0.5 mmol 1,2,4-trivinylcyclohexane (TVCH) 81 mg in a flask. 0.029 mmol tris(o-methylphenyl)phosphine 14 mg, 0.018 mmol palladium acetate 7 mg, 0.3 ml triethylamine, 1 ml acetonitrile, stirred at 85 degrees in an argon atmosphere for 24 hours. Cool, spin-dry solvent. With neutral alumina to quickly pass the column, the solvent was dried to obtain a yellow-green solid, methanol was recrystallized, and vacuum drying was given to obtain a colorless colloidal solid with a yield of 40%. Reaction processes such as Figure 5 as shown.
[0056] The nuclear magnetic profile of benzocyclobutene-substituted triethylenecyclohexane compounds prepared in the present embodiment, as shown in Figure 6 as shown.
[0057] The benzocyclobutene substituted triethylenecyclohexane compound prepared from the present embodiment is thermally cured, and the benzocyclobutene derivative is prepared to be heat-cured resin, i.e., an organic dielectric ...
Embodiment 3
[0063] Weigh 1.65 mmol 4-bromobenzocyclobutene (BBCB) 302 mg, 0.5 mmol 1,2,4-trivinylcyclohexane (TVCH) 81 mg in a flask. 0.029 mmol tris(o-methylphenyl)phosphine 14 mg, 0.018 mmol palladium acetate 7 mg, 0.3 ml triethylamine, 1 ml acetonitrile, stirred at 85 degrees in an argon atmosphere for 24 hours. Cool, spin-dry solvent. Neutral alumina was used to quickly pass the column, the solvent was dried to obtain a yellow-green solid, methanol was recrystallized, and 168mg of yellow-green solid was obtained by vacuum drying, with a yield of 71.8%. Reaction processes such as Figure 9 as shown.
[0064] The nuclear magnetic profile of benzocyclobutene-substituted triethylenecyclohexane compounds prepared in the present embodiment, as shown in Figure 10 as shown.
[0065] The benzocyclobutene substituted triethylenecyclohexane compound prepared from the present embodiment is thermally cured, and the benzocyclobutene derivative is prepared to be heat-cured resin, i.e., an organic dielect...
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