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Method for preparing 1,4-bis(2,6-di-nitryl-4-trifluoromethyl phenoxy)-2,5 bi-utylbenzene

A technology of trifluoromethylphenoxy and trifluoromethylhalogenated benzene, which is applied in the field of preparation of aromatic organic compounds, can solve the problems of unpublished patents or literature reports, and achieve less types of use and less waste , the effect of convenient recycling

Inactive Publication Date: 2008-09-24
DONGHUA UNIV
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  • Abstract
  • Description
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  • Application Information

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Problems solved by technology

[0004] But the preparation method of 1,4-bis(2,6-dinitro-4-trifluoromethylphenoxy)-2,5-di-tert-butylbenzene, there is no published patent or literature report yet

Method used

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  • Method for preparing 1,4-bis(2,6-di-nitryl-4-trifluoromethyl phenoxy)-2,5 bi-utylbenzene
  • Method for preparing 1,4-bis(2,6-di-nitryl-4-trifluoromethyl phenoxy)-2,5 bi-utylbenzene
  • Method for preparing 1,4-bis(2,6-di-nitryl-4-trifluoromethyl phenoxy)-2,5 bi-utylbenzene

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] 22.2 grams (0.10 moles) of 2,5-di-tertbutylhydroquinone, 54.1 grams (0.20 moles) of 2,6-dinitro-4-trifluoromethylchlorobenzene, 110.4 grams (0.80 moles) Potassium carbonate, 1000 milliliters of N, N-dimethylformamide, 50 milliliters of benzene and 50 milliliters of toluene 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 was added with water to precipitate a solid product, washed 2 to 3 times with hot water, and dried to obtain 64.3 grams of 1,4-bis(2,6-dinitro-4-trifluoromethylphenoxy)- 2,5-Di-tert-butylbenzene crystal product with a purity of 99.7%. According to the actual amount of 1,4-bis(2,6-dinitro-4-trifluoromethylphenoxy)-2,5-di-tert-butylbenzene and the theoretical amount (69.0 grams), the calculation of 1 , the yield of 4-bis(2,6-dinitro-4-trifluoromethylphenoxy)-2,5-di-tert-butylbenzene was 93.2%.

Embodiment 2

[0030] 22.2 grams (0.10 moles) of 2,5-di-tertbutyl hydroquinone, 69.3 grams (0.22 moles) of 2,6-dinitro-4-trifluoromethylbromobenzene, 10.0 grams (0.10 moles) Potassium bicarbonate, 55.2 grams (0.40 moles) of potassium carbonate, 650 milliliters of N-methyl-2-pyrrolidone, 50 milliliters of N, N-dimethylacetamide and 1000 milliliters of toluene were put into the reactor, stirred, heated to reflux After reacting with water for 12 hours, concentrate the reaction solution, recover the solvent for recycling, cool the reactant system, add water, and precipitate a solid product, wash with hot water 2 to 3 times, and dry to obtain 61.5 grams of 1,4-bis(2,6 - A crystalline product of dinitro-4-trifluoromethylphenoxy)-2,5-di-tert-butylbenzene with a purity of 99.8%. According to the actual amount of 1,4-bis(2,6-dinitro-4-trifluoromethylphenoxy)-2,5-di-tert-butylbenzene and the theoretical amount (69.0 grams), the calculation of 1 , the yield of 4-bis(2,6-dinitro-4-trifluoromethylphenox...

Embodiment 3

[0032] 22.2 grams (0.10 moles) of 2,5-di-tertbutylhydroquinone, 54.1 grams (0.20 moles) of 2,6-dinitro-4-trifluoromethylchlorobenzene, 10.6 grams (0.10 moles) Sodium carbonate, 40 ml of N-methyl-2-pyrrolidone, 700 ml of benzene and 100 ml of dichlorobenzene were put into the reaction kettle, stirred, heated to reflux and separated from water for 13 hours, the reaction solution was concentrated, and the solvent was recovered for recycling , cooling the reactant system, adding water, the solid product was separated out, washed 2 to 3 times with hot water, and dried to obtain 51.4 grams of 1,4-bis(2,6-dinitro-4-trifluoromethylphenoxy) -2,5-di-tert-butylbenzene crystal product with a purity of 99.2%, according to the actual obtained 1,4-bis(2,6-dinitro-4-trifluoromethylphenoxy)-2,5 - Amount and theoretical yield (69.0 g) of di-tert-butylbenzene, calculated to give 1,4-bis(2,6-dinitro-4-trifluoromethylphenoxy)-2,5-di-tert-butyl The yield of phenylbenzene was 74.5%.

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Abstract

The present invention relates to a preparation method of 1, 4-bi (2, 6-dinitro-4-trifluoromethyl phenoxy)-2, 5-di-tert-butyl benzene. The preparation method comprises the following steps: (1) 2, 5-di-tert-butyl hydroquinone and 2, 6-dinitro-4-trifluoromethyl halogenated benzene with the molar ratio of from 1.0 : 2.0 to 2.2 are put in the system of salt-forming agent and organic solvent for 6 to 18 hours with heated reflux reaction and water diversion; (2) the reaction solution is concentrated; the reaction system is cooled; water is added; solid products are separated, filtered, washed and dried to prepare the crystals of the 1, 4-bi (2, 6-dinitro-4-trifluoromethyl phenoxy)-2, 5-di-tert-butyl benzene. The preparation method has the advantages of simple operation, high yield of the product, high purity of the product, convenient recovery of the solvent that can be used repeatedly, less three-waste, less environmental pollution, and suitability for the industrial production.

Description

technical field [0001] The invention belongs to the field of preparation of aromatic organic compounds, in particular to 1,4-bis(2,6-dinitro-4-trifluoromethylphenoxy)-2,5-di-tert-butylbenzene method of preparation. 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] 1,4-bis(2,6-dinitro-4-trifluoromethylphenoxy)-2,5-di-tert-butylbenzene is one of the important raw materials for the synthesis of highly branched aromatic polyimide monomers First, it is an impor...

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 虞鑫海徐永芬
Owner DONGHUA UNIV
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