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Method for preparing 1,3,5-tri(2,4-dinitrophenoxy) benzene

A technology of dinitrophenoxy and dinitro, which is applied in 1 field to achieve the effects of simple operation, convenient recycling, and less waste

Inactive Publication Date: 2011-06-08
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] But the preparation method of 1,3,5-three (2,4-dinitrophenoxy) benzene, there is no published patent or bibliographical information yet at present

Method used

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  • Method for preparing 1,3,5-tri(2,4-dinitrophenoxy) benzene
  • Method for preparing 1,3,5-tri(2,4-dinitrophenoxy) benzene
  • Method for preparing 1,3,5-tri(2,4-dinitrophenoxy) benzene

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Experimental program
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Effect test

Embodiment 1

[0027] 12.6 grams (0.10 moles) of 1,3,5-pyrogallol, 64.8 grams (0.32 moles) of 2,4-dinitrochlorobenzene, 110.4 grams (0.80 moles) of potassium carbonate, 700 milliliters of N, N- Put dimethylformamide and 180 ml of toluene into the reaction kettle, stir, heat and reflux for water separation for 18 hours, concentrate the reaction solution, recover the solvent for recycling, cool the reactant system, add water, precipitate a solid product, wash and dry , obtain 58.2 grams of 1,3,5-three (2,4-dinitrophenoxy) benzene crystal products, the purity is 99.0%, according to the actual acquisition of 1,3,5-three (2,4-dinitrophenoxy) The yield of 1,3,5-tri(2,4-dinitrophenoxy)benzene was calculated to be 93.2%.

Embodiment 2

[0029] 12.6 grams (0.10 moles) of 1,3,5-pyrogallol, 0.32 moles of 2,4-dinitrobromobenzene, 55.2 grams (0.40 moles) of potassium carbonate, 150 milliliters of N,N-dimethylethane Amide and 15 milliliters of dimethylbenzene were put into the reaction kettle, stirred, heated to reflux and separated from water for 6 hours, concentrated the reaction solution, recovered the solvent for recycling, cooled the reactant system, added water, precipitated a solid product, washed and dried to obtain 1 , 3,5-tris(2,4-dinitrophenoxy)benzene crystal product, according to the actual amount and theoretical amount of 1,3,5-tris(2,4-dinitrophenoxy)benzene obtained (62.4 g), the calculated yield of 1,3,5-tris(2,4-dinitrophenoxy)benzene was 87.3%.

Embodiment 3

[0031] 12.6 grams (0.10 moles) of 1,3,5-pyrroglucinol, 0.30 moles of 2,4-dinitrochlorobenzene, 10.6 grams (0.10 moles) of sodium carbonate, 80 milliliters of N-methyl-2-pyrrolidone and 30 milliliters of dichlorobenzene were put into a reaction kettle, stirred, heated to reflux and separated from water for 16 hours, concentrated the reaction solution, recovered the solvent for recycling, cooled the reactant system, added water, precipitated a solid product, washed, dried, and obtained 1,3,5-tris(2,4-dinitrophenoxy)benzene crystal product, according to the actual amount of 1,3,5-tris(2,4-dinitrophenoxy)benzene obtained and Theoretical yield (62.4 g), the calculated yield of 1,3,5-tris(2,4-dinitrophenoxy)benzene was 88.1%.

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Abstract

The invention relates to a method for preparing 1, 3, 5-three(-2, 4 dinitrophenoxy) benzene, which comprises the steps that: (1) 1, 3, 5-phloroglucin and 2, 4-dinitrohalobenzenes with a molar ratio ranging from 1.0 : 3.0 to 1.0 : 3.2 are subject to a heat refluxing and water diversion reaction for 6 to 18 hours in a system comprising the salt forming agents and organic solvents; (2) the reaction solution is concentrated, the reactant system is cooled and the water is added in the reactant system so as to precipitate the solid product; the obtained solutions are filtered, the obtained productsare washed and dried so as to, obtain 1, 3, 5-three (-2, 4 dinitrophenoxy) benzene. The invention has simple operations and high product yield and purity, the solvents can be conveniently recycled and can be repeatedly used with few wastes, and the invention is environmentally friendly and suitable for industrialized production.

Description

technical field [0001] The invention belongs to the field of preparation of aromatic organic compounds, in particular to a preparation method of 1,3,5-tris(2,4-dinitrophenoxy)benzene. Background technique [0002] Aromatic polyimide has excellent thermal stability, chemical stability, nuclear radiation resistance, excellent mechanical properties, electrical properties and resistance to organic solvents, and has been widely used in aerospace, electronic microelectronics, electrical and other fields . Because of its high temperature resistance, high strength, corrosion resistance, good insulation, and simple film forming process, it is an excellent functional material that can meet the performance requirements of LCD (liquid crystal display). [0003] 1,3,5-tris(2,4-dinitrophenoxy)benzene is one of the important raw materials for the synthesis of highly branched aromatic polyimide monomers, that is, an important raw material for aromatic polyvalent primary amines. Aromatic p...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C205/38C07C201/12
CPCY02P20/582
Inventor 虞鑫海
Owner DONGHUA UNIV
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