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Preparation of 1,4-bis(2,4- dinitrophenoxy)-2,3,5- trimethylbenzene

A technology of dinitrophenoxy and trimethylbenzene, applied in 1 field, achieves the effects of high yield and purity, few types of use, and simple operation

Inactive Publication Date: 2011-06-22
DONGHUA UNIV +1
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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(2,4-dinitrophenoxy)-2,3,5-trimethylbenzene, there is no published patent or literature report yet

Method used

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  • Preparation of 1,4-bis(2,4- dinitrophenoxy)-2,3,5- trimethylbenzene
  • Preparation of 1,4-bis(2,4- dinitrophenoxy)-2,3,5- trimethylbenzene
  • Preparation of 1,4-bis(2,4- dinitrophenoxy)-2,3,5- trimethylbenzene

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Experimental program
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Effect test

Embodiment 1

[0026] 15.2 grams (0.10 moles) of 2,3,5-trimethylhydroquinone, 44.6 grams (0.22 moles) of 2,4-dinitrochlorobenzene, 110.4 grams (0.80 moles) of potassium carbonate, 1216 milliliters of N , N-dimethylformamide and 130 milliliters of benzene were put into the reaction kettle, stirred, heated to reflux and separated from water for 18 hours, concentrated the reaction solution, recovered the solvent for recycling, cooled the reactant system, added water, and precipitated a solid product. Wash 2 to 3 times with hot water, dry to obtain 45.1 grams of 1,4-bis(2,4-dinitrophenoxy)-2,3,5-trimethylbenzene with a purity of 99.4%. The amount and theoretical amount (48.4 g) of 1,4-bis(2,4-dinitrophenoxy)-2,3,5-trimethylbenzene obtained was calculated to give 1,4-bis(2,4 The yield of -dinitrophenoxy)-2,3,5-trimethylbenzene was 93.2%.

Embodiment 2

[0028] 15.2 grams (0.10 moles) of 2,3,5-trimethylhydroquinone, 54.4 grams (0.22 moles) of 2,4-dinitrobromobenzene, 55.2 grams (0.40 moles) of potassium carbonate, 10.6 grams ( 0.10 mole) of sodium carbonate, 600 milliliters of N, N-dimethylacetamide, 160 milliliters of benzene and 30 milliliters of dimethylbenzene were put into the reaction kettle, stirred, and after heating and reflux water separation reaction for 6 hours, the reaction solution was concentrated, and the solvent was recovered to Recycle, cool the reactant system, add water, precipitate a solid product, wash with hot water 2 to 3 times, and dry to obtain 37.8 grams of 1,4-bis(2,4-dinitrophenoxy)-2,3, 5-trimethylbenzene, the purity is 99.5%, according to the actual amount and theoretical amount (48.4 grams), the calculated yield of 1,4-bis(2,4-dinitrophenoxy)-2,3,5-trimethylbenzene was 78.2%.

Embodiment 3

[0030] 15.2 grams (0.10 moles) of 2,3,5-trimethylhydroquinone, 40.5 grams (0.20 moles) of 2,4-dinitrochlorobenzene, 10.6 grams (0.10 moles) of sodium carbonate, 76 milliliters of N -Methyl-2-pyrrolidone, 100 milliliters of benzene and 52 milliliters of dichlorobenzene were put into the reaction kettle, stirred, heated to reflux and separated from water for 12 hours, concentrated the reaction solution, recovered the solvent for recycling, cooled the reactant system, Add water, separate out solid product, wash 2~3 times with hot water, dry, obtain 36.6 grams of 1,4-bis(2,4-dinitrophenoxy)-2,3,5-trimethylbenzene, purity Be 99.7%, according to the amount of 1,4-bis(2,4-dinitrophenoxy)-2,3,5-trimethylbenzene actually obtained and theoretical yield (48.4 grams), calculate 1, The yield of 4-bis(2,4-dinitrophenoxy)-2,3,5-trimethylbenzene was 75.6%.

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Abstract

The invention relates to a method to prepare 1,4-bi(2,4-binitro-4-dinitro-phenoxyl) -2,3,5-trimethylbenzene, including the following steps: (1), 2,3,5-trimethyl-hydroquinone and 2,4-binitro-halogenated benzene based on molar ratio of 1.0:2.0-2.2 are heated to reflux and react for 6-18 hours in a system with salt forming agent and organic solvent;(2) after reaction, the solution is concentrated and cooled, and then water is added to separate out the solid product, after that the solution is filtrated, washed and dried, getting 1,4-bi(2,4-binitro-4-dinitro-phenoxyl)-2,3,5-trimethylbenzene crystalloid. The method is simple in operation with high yield and the product is high in purity; the solvent is convenient to recycle and can be used repeatedly; with little wastes(gas, liquid and solid)and being environment-friendly, the method is applicable to 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 1,4-bis(2,4-dinitrophenoxy)-2,3,5-trimethylbenzene. 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(2,4-dinitrophenoxy)-2,3,5-trimethylbenzene is one of the important raw materials for the synthesis of aromatic polyimide monomers, that is, aromatic polyvalent primary amines important raw materials. Aroma...

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 虞鑫海陈梅芳陈健丽刘斌
Owner DONGHUA UNIV
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