Method for preparing 1, 3, 5-tri (4-aminophenoxy) benzene

A technology of aminophenoxy and trichlorobenzene, which is applied in chemical instruments and methods, preparation of organic compounds, preparation of aminohydroxyl compounds, etc., can solve the problems of inapplicability to mass production, low production efficiency, and low yield of products, etc. problems, to achieve the effect of high product yield, lower production cost, and simple operation steps

Active Publication Date: 2021-10-15
天津众泰材料科技有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In the above-mentioned two prior art, 1,3,5-tris(4-aminophenoxy)benzene is prepared by two-step reaction, and the product yield is low, the production cost is high, and the production efficiency is low, so it is not suitable for batch production. chemical production

Method used

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  • Method for preparing 1, 3, 5-tri (4-aminophenoxy) benzene

Examples

Experimental program
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Effect test

Embodiment 1

[0028] Add 32.7g of 4-hydroxyaniline to the reaction flask, add it to 350g of sulfolane, add 15g of cesium hydroxide in batches under mechanical stirring, then raise the temperature to 60°C, slowly add 18g of trichlorobenzene, 1.5g of cesium fluoride, and then Raise the temperature to 130°C and keep the reaction at this temperature. After the raw materials have reacted completely, the reaction solution is cooled to 60°C and filtered with diatomaceous earth. The filter cake is washed with sulfolane, and half of the solvent is recovered from the filtrate under reduced pressure. , add water to the reaction solution, cool down to below 10°C in an ice bath under stirring, filter, wash with water, and dry in a vacuum oven to obtain 1,3,5-tris(4-aminophenoxy)benzene, 32.7g, off-white solid , yield 81.95%.

Embodiment 2

[0030] Add 32.8g of 4-hydroxyaniline to the reaction flask, add it to 500g of sulfolane, add 18g of cesium hydroxide in batches under mechanical stirring, then raise the temperature to 60°C, slowly add 18g of trichlorobenzene, 4.5g of cesium fluoride, and then Raise the temperature to 160°C and keep the reaction at this temperature. After the reaction of the raw materials is complete, the reaction solution is cooled to 60°C and filtered with diatomaceous earth, the filter cake is washed with sulfolane, half of the solvent is recovered from the filtrate under reduced pressure, water is added to the reaction solution, and stirred Lower the temperature in an ice bath to below 10°C, filter, wash with water, and dry in a vacuum oven to obtain 1,3,5-tris(4-aminophenoxy)benzene, 37.4 g, off-white solid, with a yield of 93.73%.

Embodiment 3

[0032] Add 32.9g of 4-hydroxyaniline to the reaction flask, add it to 750g of sulfolane, add 19.5g of cesium hydroxide in batches under mechanical stirring, then raise the temperature to 60°C, slowly add 18g of trichlorobenzene, 7.6g of cesium fluoride, After that, the temperature was raised to 160°C, and the reaction was maintained at this temperature. After the raw materials were completely reacted, the reaction solution was cooled to 60°C and filtered with diatomaceous earth. The filter cake was washed with sulfolane, and half of the solvent was recovered from the filtrate under reduced pressure, and water was added to the reaction solution. Cool down to below 10°C in an ice bath with stirring, filter, wash with water, and dry in a vacuum oven to obtain 1,3,5-tris(4-aminophenoxy)benzene, 37.5 g, off-white solid, yield 93.98%.

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Abstract

The invention provides a method for preparing 1, 3, 5-tri (4-aminophenoxy) benzene, the method comprises the following steps: mixing 4-hydroxyaniline with an organic solvent, and adding an alkaline substance to obtain a mixed solution; adding sym-trichlorobenzene and a catalyst into the mixed solution, and heating until the reaction is complete; the preparation method is a one-step reaction, the operation steps are simple, the reaction conditions are mild, the product yield is high, the industrial application prospect is achieved, the solvent in the reaction liquid after the reaction can be recycled, reutilization can be achieved, and the production cost is reduced.

Description

technical field [0001] The invention belongs to the field of polyimide 5G material preparation technology, and in particular relates to a method for preparing 1,3,5-tris(4-aminophenoxy)benzene. Background technique [0002] 1,3,5-tris(4-aminophenoxy)benzene, as an amino-containing monomer, is mainly used in semiconductor materials and mobile phone antenna materials after polymerization with acid anhydrides. [0003] The invention patent with the application number CN02137746.4 discloses 1,3,5-tris(4-aminophenoxy)benzene and its preparation method, using triphenol and p-chloronitrobenzene as raw materials, through two steps of substitution and reduction The reaction is obtained, and the two-step yield is 20%; [0004] In [RSC Advances.6(13), 10683-10696, 2016], LIN Ruey-Chorng used trisphenol and p-fluoronitrobenzene as raw materials, potassium carbonate as base, and obtained 1,3,5-tri( 4-aminophenoxy)benzene, the yield of the second step is 75%. [0005] In the above-ment...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C217/90C07C213/06
CPCC07C213/06C07C217/90
Inventor 栗晓东
Owner 天津众泰材料科技有限公司
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