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Method for preparing 4,4', di(2,6-dinitro-4-trifluoromethyl phenoxy)diphenyl ether

A technology of trifluoromethylphenoxy and dihydroxydiphenyl ether, which is applied in 4 fields and achieves the effects of simple operation, high yield and purity, and low investment

Inactive Publication Date: 2008-10-22
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 4,4'-bis(2,6-dinitro-4-trifluoromethylphenoxy) diphenyl ether, there is no published patent or bibliographical information yet at present

Method used

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  • Method for preparing 4,4', di(2,6-dinitro-4-trifluoromethyl phenoxy)diphenyl ether
  • Method for preparing 4,4', di(2,6-dinitro-4-trifluoromethyl phenoxy)diphenyl ether

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Experimental program
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Effect test

Embodiment 1

[0027] 20.2 grams (0.10 moles) of 4,4'-dihydroxydiphenyl ether, 59.5 grams (0.22 moles) of 2,6-dinitro-4-trifluoromethylchlorobenzene, 110.4 grams (0.80 moles) of potassium carbonate , 1200 milliliters of N, N-dimethylformamide, 180 milliliters of benzene and 60 milliliters of toluene were put into the reaction kettle, stirred, heated to reflux and separated from water for 10 hours, concentrated the reaction solution, recovered the solvent for recycling, and cooled the reactant system, add water, precipitate a solid product, wash 2 to 3 times with hot water, and dry to obtain 64.8 grams of 4,4'-bis(2,6-dinitro-4-trifluoromethylphenoxy)diphenyl Ether crystal product with a purity of 99.7%, according to the actual amount of 4,4'-bis(2,6-dinitro-4-trifluoromethylphenoxy)diphenyl ether and the theoretical amount (67.0 grams), The calculated yield of 4,4'-bis(2,6-dinitro-4-trifluoromethylphenoxy)diphenyl ether was 96.7%.

Embodiment 2

[0029] 20.2 grams (0.10 moles) of 4,4'-dihydroxydiphenyl ether, 69.3 grams (0.22 moles) of 2,6-dinitro-4-trifluoromethylbromobenzene, 10.0 grams (0.10 moles) of bicarbonate Potassium, 10.6 grams (0.10 moles) of sodium carbonate, 55.2 grams (0.40 moles) of potassium carbonate, 200 milliliters of N-methyl-2-pyrrolidone, 600 milliliters of N, N-dimethylacetamide, 100 milliliters of benzene and 30 milliliters of di Put toluene in the reaction kettle, stir, heat and reflux for water separation for 15 hours, concentrate the reaction solution, recover the solvent for recycling, cool the reactant system, add water, precipitate a solid product, wash with hot water 2 to 3 times, and dry. Obtain 61.2 grams of 4,4'-bis(2,6-dinitro-4-trifluoromethylphenoxy) diphenyl ether crystal product, the purity is 99.6%, according to the actual 4,4'-bis(2 , the amount of 6-dinitro-4-trifluoromethylphenoxy) diphenyl ether and the theoretical amount (67.0 g), calculated 4,4'-bis(2,6-dinitro-4-tri The y...

Embodiment 3

[0031] 20.2 grams (0.10 moles) of 4,4'-dihydroxydiphenyl ether, 54.1 grams (0.20 moles) of 2,6-dinitro-4-trifluoromethylchlorobenzene, 10.6 grams (0.10 moles) of sodium carbonate , 110 milliliters of N-methyl-2-pyrrolidone, 2000 milliliters of benzene and 200 milliliters of dichlorobenzene were put into the reaction kettle, stirred, heated to reflux and separated from water for 10 hours, concentrated the reaction solution, recovered the solvent for recycling, cooled The reactant system was added with water to precipitate a solid product, washed 2 to 3 times with hot water, and dried to obtain 55.2 grams of 4,4'-bis(2,6-dinitro-4-trifluoromethylphenoxy) di Diphenyl ether crystal product, the purity is 99.7%, according to the amount and theoretical yield of 4,4'-bis(2,6-dinitro-4-trifluoromethylphenoxy)diphenyl ether actually obtained (67.0 g ), the calculated yield of 4,4'-bis(2,6-dinitro-4-trifluoromethylphenoxy)diphenyl ether was 82.4%.

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Abstract

The invention relates to a preparation method of 4, 4'-bis (2, 6-dinitro-4-trifluoromethyl phenoxy) diphenyl ether, including the following steps: (1) in salifying agents and the organic solvent system, 4, 4'-dihydroxy diphenyl ether and 2, 6-dinitro-4-trifluoromethyl halogeno benzene with a molar ratio of 1.0:2.0 to 2.2 carry on heating reflux water reaction for six to eighteen hours; (2) the reaction liquid is condensed; the reactant system is cooled; water is added to precipitate solid product; after filtered, washed and dried, the crystal of 4, 4'- bis(2, 6-dinitro-4 trifluoromethyl phenoxy) diphenyl ether is obtained. The method of the invention has the advantages of simple operation, high yield and purity of products, convenient recovery of solvent, repeated use, fewer three wastes, friendly environment and applicable to the industrial production.

Description

technical field [0001] The invention belongs to the field of preparation of aromatic organic compounds, in particular to a preparation method of 4,4'-bis(2,6-dinitro-4-trifluoromethylphenoxy)diphenyl ether. 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] 4,4'-bis(2,6-dinitro-4-trifluoromethylphenoxy)diphenyl ether is one of the important raw materials for the synthesis of highly branched aromatic polyimide monomers, that is, aromatic polyimide An importan...

Claims

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Application Information

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IPC IPC(8): C07C205/38C07C201/12
CPCY02P20/582
Inventor 虞鑫海
Owner DONGHUA UNIV
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