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Synthetic method of 4-vinylbenzocyclobutene

A technology of bromobenzocyclobutene and vinylbenzene is applied in the synthesis field of 4-vinylbenzocyclobutene, can solve the problems of low comprehensive yield, complicated operation, harsh ultra-low temperature conditions, etc., and achieves simple process, Simple operation and low cost effect

Active Publication Date: 2017-02-15
绵阳高新区达高特科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among them, 4-vinylbenzocyclobutene is one of the important monomer materials of benzocyclobutene resin, which has good applications in the fields of insulation, composite materials, biomedical and packaging materials, but currently Its synthesis method is mainly as figure 1 As shown, it is a multi-step reaction, and the synthesis method requires harsh ultra-low temperature conditions, the operation is complicated, and the overall yield is low

Method used

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  • Synthetic method of 4-vinylbenzocyclobutene

Examples

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Embodiment 1

[0023] A kind of synthetic method of 4-vinyl benzocyclobutene, comprises the steps: add the solvent that dissolves potassium carbonate in autoclave, then 4-bromo benzocyclobutene and catalyst are added in solvent, close still cover Use nitrogen to replace the air in the autoclave three times, then feed ethylene gas to make the reaction pressure reach 1MPa, seal and heat up to 70°C, stir and react for 5 hours, the pressure drops to 0.5MPa, stop heating, and obtain the reaction solution. Separate the phases to obtain an oil phase and an aqueous phase; the aqueous phase was extracted twice with ether, and the obtained ether phase was combined with the oil phase, then washed once with deionized water and saturated sodium chloride solution, and dried over anhydrous sodium sulfate for 4 hours Above, after drying, the solvent was removed by rotary evaporation, concentrated into a light yellow oily liquid, and purified by vacuum distillation using a high vacuum oil pump, and the fracti...

Embodiment 2

[0025] A kind of synthetic method of 4-vinyl benzocyclobutene, comprises the steps: add the solvent that dissolves potassium carbonate in autoclave, then 4-bromo benzocyclobutene and catalyst are added in solvent, close still cover Use nitrogen to replace the air in the autoclave three times, then feed ethylene gas to make the reaction pressure reach 10MPa, seal and heat up to 90°C, stir and react for 8 hours, the pressure drops to 3MPa, stop heating, and obtain the reaction solution. phase to obtain an oil phase and an aqueous phase; the aqueous phase was extracted twice with ether, and the obtained ether phase was combined with the oil phase, then washed once with deionized water and saturated sodium chloride solution, and dried over anhydrous sodium sulfate for more than 4 hours After drying, the solvent was removed by rotary evaporation, concentrated into a light yellow oily liquid, and purified by vacuum distillation using a high vacuum oil pump, and the fractions at 75-80...

Embodiment 3

[0027] A kind of synthetic method of 4-vinyl benzocyclobutene, comprises the steps: add the solvent that dissolves potassium carbonate in autoclave, then 4-bromo benzocyclobutene and catalyst are added in solvent, close still cover Use nitrogen to replace the air in the autoclave three times, then feed ethylene gas to make the reaction pressure reach 4MPa, seal and heat up to 80°C, stir and react for 6 hours, the pressure drops to 2.5MPa, stop heating, and obtain the reaction solution. Separate the phases to obtain an oil phase and an aqueous phase; the aqueous phase was extracted twice with ether, and the obtained ether phase was combined with the oil phase, then washed once with deionized water and saturated sodium chloride solution, and dried over anhydrous sodium sulfate for 4 hours Above, after drying, the solvent was removed by rotary evaporation, concentrated into a light yellow oily liquid, and purified by vacuum distillation using a high vacuum oil pump, and the fracti...

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Abstract

The invention discloses a synthetic method of 4-vinylbenzocyclobutene. The synthetic method comprises following steps: 4-bromobenzocyclobutene and a catalyst are added into a solvent containing an acid-binding agent; an obtained mixture is delivered into a reaction system with nitrogen atmosphere, and ethylene gas is delivered into the reaction system until reaction pressure is increased to 1 to 10MPa; sealing and heating stirring reaction are carried out so as to obtain a reaction solution, and the reaction solution is subjected to treatment so as to obtain 4-vinylbenzocyclobutene. According to the synthetic method, 4-bromobenzocyclobutene is taken as a raw material, and one step reaction is carried out in an autoclave so as to obtain target product 4-vinylbenzocyclobutene; cost is low; technology is simple; and operation is convenient.

Description

technical field [0001] The invention relates to a method for synthesizing 4-vinylbenzocyclobutene, in particular to a method for synthesizing 4-vinylbenzocyclobutene by one-step reaction of 4-bromobenzocyclobutene and ethylene gas. Background technique [0002] Benzocyclobutene compounds are a class of highly reactive compounds, which can be modified by copolymerization and blending of different monomers to synthesize various high-performance resin materials. Benzocyclobutene resin is a new type of polymer material with excellent high temperature resistance, dielectric properties and hydrophobic properties. It can be used on printed circuit boards, and can also be used as an interlayer insulating material for integrated circuits. The miniaturization, high speed and densification of microelectronic components urgently require new polymer dielectric materials, and require easy processing, good planarization behavior, low dielectric constant and good mechanical properties. Be...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C1/26C07C7/04C07C13/44
CPCC07C1/26C07C7/04C07C13/44
Inventor 冯毅汪云峰
Owner 绵阳高新区达高特科技有限公司
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