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Method for preparing 3,5-di(2,4-dinitrophenoxy)trifluorotoluene

A technology of dinitrophenoxy and hydroxytrifluorotoluene is applied in 3 fields, can solve the problems such as no patents, literature reports and the like in the preparation method, and achieves the advantages of easy popularization and application, high product yield and purity, and less three wastes. Effect

Inactive Publication Date: 2008-08-06
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] 3,5-bis(2,4-dinitrophenoxy)benzotrifluoride is an important raw material for aromatic polyvalent primary amines, but its preparation method has no patents or literature reports

Method used

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  • Method for preparing 3,5-di(2,4-dinitrophenoxy)trifluorotoluene
  • Method for preparing 3,5-di(2,4-dinitrophenoxy)trifluorotoluene

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Experimental program
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Effect test

Embodiment 1

[0027] 17.8 grams (0.10 moles) of 3,5-dihydroxybenzotrifluoride, 44.6 grams (0.22 moles) of 2,4-dinitrochlorobenzene, 110.4 grams (0.80 moles) of potassium carbonate, 700 milliliters of N, N-di Methylformamide and 180 ml of toluene were put into the reaction kettle, stirred, heated to reflux and separated from water for 18 hours, then concentrated the reaction solution, recovered the solvent for recycling, cooled the reactant system, added water, precipitated a solid product, washed with hot water 2~3 times, dry, obtain 48.6 grams of 3,5-bis(2,4-dinitrophenoxy)benzotrifluorotoluene crystal product, the purity is 99.0%, obtain 3,5-bis(2, The amount and theoretical amount (51.0 grams) of 4-dinitrophenoxy)benzotrifluoride, the calculated yield of 3,5-bis(2,4-dinitrophenoxy)benzotrifluoride is 95.3% .

Embodiment 2

[0029] 17.8 grams (0.10 moles) of 3,5-dihydroxytrifluorotoluene, 54.4 grams (0.22 moles) of 2,4-dinitrobromobenzene, 55.2 grams (0.40 moles) of potassium carbonate, 150 milliliters of N, N-two Methyl acetamide and 15 milliliters of xylene were put into the reaction kettle, stirred, heated and refluxed for water separation for 3 hours, concentrated the reaction solution, recovered the solvent for recycling, cooled the reactant system, added water, and precipitated a solid product, washed with hot water Washed 2 to 3 times and dried to obtain 31.8 grams of 3,5-bis(2,4-dinitrophenoxy)trifluorotoluene crystal product with a purity of 99.1%. According to actual conditions, 3,5-bis(2, The amount and theoretical amount (51.0 grams) of 4-dinitrophenoxy)benzotrifluoride, the calculated yield of 3,5-bis(2,4-dinitrophenoxy)benzotrifluoride is 62.3% .

Embodiment 3

[0031] 17.8 grams (0.10 moles) of 3,5-dihydroxybenzotrifluoride, 40.5 grams (0.20 moles) of 2,4-dinitrochlorobenzene, 10.6 grams (0.10 moles) of sodium carbonate, 96 milliliters of N-methyl- 2-pyrrolidone and 36 milliliters of dichlorobenzene were put into the reaction kettle, stirred, heated to reflux and separated from water for 16 hours, the reaction solution was concentrated, the solvent was recovered for recycling, the reactant system was cooled, water was added, and a solid product was precipitated, and heated Washed with water for 2 to 3 times, dried to obtain 41.5 grams of 3,5-bis(2,4-dinitrophenoxy)benzotrifluorotoluene crystal product with a purity of 99.3%. According to the actual obtained 3,5-bis( 2, the amount of 4-dinitrophenoxy) trifluorotoluene and theoretical output (51.0 grams), calculate the yield of 3,5-two (2,4-dinitrophenoxy) trifluorotoluene as 81.3%.

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Abstract

The invention relates to a preparation method of 3, 5-bi-(2, 4-dinitrophenoxy) benzotrifluoride, which comprises (1), heating, refluxing and water segregating for 3-18h to treat 3, 5-dihydroxy benzotrifluoride and 2, 4-dinitro halogenated benzene at the mol ratio of 1.0:2.0-2.2, in the system of salt forming agent and organic solvent, (2), condensing reaction liquid, cooling reactant system, adding water, precipitating solid product, filtering, washing and drying to obtain 3, 5-bi-(2, 4-dinitrophenoxy) benzotrifluoride. The preparation method of 3, 5-bi-(2, 4-dinitrophenoxy) benzotrifluoride has simple operation, high yield and purity, easily recovered and circulated solvent, less generation of three wastes, environment-friend property and application in 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 3,5-bis(2,4-dinitrophenoxy)benzotrifluoride. 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] 3,5-bis(2,4-dinitrophenoxy)benzotrifluoride 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....

Claims

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Application Information

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