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Method for preparing 1,4-di(2,6-dinitryl-4-trifluoromethyl phenoxy)-2,6-dimethyl benzene

A technology of trifluoromethylphenoxy and trifluoromethylhalogenated benzene, which is applied in the field of preparation of aromatic organic compounds, can solve problems such as patents or literature reports, and achieve fewer types of use, easy promotion and application, and product collection. The effect of high rate and purity

Inactive Publication Date: 2008-10-29
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 1,4-bis(2,6-dinitro-4-trifluoromethylphenoxy)-2,6-dimethylbenzene, there is no published patent or literature report yet

Method used

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  • Method for preparing 1,4-di(2,6-dinitryl-4-trifluoromethyl phenoxy)-2,6-dimethyl benzene
  • Method for preparing 1,4-di(2,6-dinitryl-4-trifluoromethyl phenoxy)-2,6-dimethyl benzene

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] 13.8 grams (0.10 moles) of 2,6-dimethylhydroquinone, 54.1 grams (0.20 moles) of 2,6-dinitro-4-trifluoromethylchlorobenzene, 110.4 grams (0.80 moles) of carbonic acid Potassium, 800 milliliters of N, N-dimethylformamide and 80 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, and added water , a solid product was precipitated, washed 2 to 3 times with hot water, and dried to obtain 51.7 grams of 1,4-bis(2,6-dinitro-4-trifluoromethylphenoxy)-2,6-bis The methylbenzene crystal product has a purity of 99.7%, according to the actual amount of 1,4-bis(2,6-dinitro-4-trifluoromethylphenoxy)-2,6-dimethylbenzene and Theoretical amount (60.6 g), the calculated yield of 1,4-bis(2,6-dinitro-4-trifluoromethylphenoxy)-2,6-dimethylbenzene is 85.3%.

Embodiment 2

[0029] 13.8 grams (0.10 moles) of 2,6-dimethylhydroquinone, 69.3 grams (0.22 moles) of 2,6-dinitro-4-trifluoromethylbromobenzene, 55.2 grams (0.40 moles) of carbonic acid Potassium, 700 milliliters of N, N-dimethylacetamide and 70 milliliters of dimethylbenzene were put into the reaction kettle, stirred, heated to reflux and split water for 12 hours, concentrated the reaction solution, recovered the solvent for recycling, cooled the reactant system, Add water to precipitate a solid product, wash with hot water 2 to 3 times, and dry to obtain 54.8 grams of 1,4-bis(2,6-dinitro-4-trifluoromethylphenoxy)-2,6-bis A crystalline product of methylbenzene with a purity of 99.5%, according to the actual obtained 1,4-bis(2,6-dinitro-4-trifluoromethylphenoxy)-2,6-dimethylbenzene Quantity and theoretical amount (60.6 grams), calculate the yield of 1,4-bis(2,6-dinitro-4-trifluoromethylphenoxy)-2,6-dimethylbenzene to be 90.5% .

Embodiment 3

[0031] 13.8 grams (0.10 moles) of 2,6-dimethylhydroquinone, 54.1 grams (0.20 moles) of 2,6-dinitro-4-trifluoromethylchlorobenzene, 10.6 grams (0.10 moles) of carbonic acid Sodium, 70 milliliters of N-methyl-2-pyrrolidone, 700 milliliters of benzene and 100 milliliters of dichlorobenzene were put into the reaction kettle, stirred, heated to reflux and separated from water for 10 hours, the reaction solution was concentrated, and the solvent was recovered for recycling. Cool the reactant system, add water, precipitate a solid product, wash 2 to 3 times with hot water, and dry to obtain 57.6 grams of 1,4-bis(2,6-dinitro-4-trifluoromethylphenoxy)- 2,6-Dimethylbenzene crystal product with a purity of 99.6%, according to the actual obtained 1,4-bis(2,6-dinitro-4-trifluoromethylphenoxy)-2,6-di The amount of methylbenzene and the theoretical output (60.6 grams), calculate the yield of 1,4-bis(2,6-dinitro-4-trifluoromethylphenoxy)-2,6-dimethylbenzene The rate is 95.1%.

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Abstract

The invention relates to a method for preparing 1,4-bis(2,6-binitro-4-trifluoromethylphenoxy)-2,6-dimethylbenzene, which comprises (1) allowing 2,6-dimethoxybenzene and 2,6-binitro-4-trifluoromethyl halogenated benzene at molar ratio of 1.0:(2.0-2.2) to react in a system of salifying agent and organic solvent while refluxing by heating for water separation for 6-18 hours; and (2) concentrating the reactant liquor, cooling the reactant system, adding water, adding water to separate out solid product, filtering, washing and drying to obtain product crystal. The method has simple process, convenient solvent recovery, repeated used of the solvent, less three wastes, environment friendliness, and suitability for industrialized production. The obtained product has high yield hand purity.

Description

technical field [0001] The invention belongs to the field of preparation of aromatic organic compounds, in particular to a kind of 1,4-bis(2,6-dinitro-4-trifluoromethylphenoxy)-2,6-dimethylbenzene 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)-2,6-dimethylbenzene is one of the important raw materials for the synthesis of highly branched aromatic polyimide monomers , which is an important raw mat...

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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