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Process for producing 1,4-dual(2,4-dinitrophenoxy) benzene

A dinitrophenoxy, dinitro technology, applied in 1 field, achieves the effects of high product yield and purity, few types of use, and convenient recovery

Inactive Publication Date: 2008-07-16
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(2,4-dinitrophenoxy)benzene does not have any published patents or bibliographical reports at present

Method used

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  • Process for producing 1,4-dual(2,4-dinitrophenoxy) benzene
  • Process for producing 1,4-dual(2,4-dinitrophenoxy) benzene

Examples

Experimental program
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Effect test

Embodiment 1

[0029] 11.0 grams (0.10 moles) of hydroquinone, 44.6 grams (0.22 moles) of 2,4-dinitrochlorobenzene, 110.4 grams (0.80 moles) of potassium carbonate, 700 milliliters of N, N-dimethylformamide and Put 180 milliliters of toluene into the reaction kettle, stir, heat and reflux for water separation and react for 18 hours, concentrate the reaction solution, recover the solvent for recycling, cool the reactant system, add water, precipitate a solid product, wash and dry to obtain 42.7 grams of yellow-brown The 1,4-bis(2,4-dinitrophenoxy)benzene crystal product has a purity of 99.8% and a melting point of 245°C. According to the actual 1,4-bis(2,4-dinitrophenoxy Base) the amount of benzene and the theoretical amount (44.2 grams), the calculated yield of 1,4-bis(2,4-dinitrophenoxy)benzene is 96.6%.

Embodiment 2

[0031] 11.0 grams (0.10 moles) of hydroquinone, 54.4 grams (0.22 moles) of 2,4-dinitrobromobenzene, 55.2 grams (0.40 moles) of potassium carbonate, 150 milliliters of N, N-dimethylacetamide and Put 15 milliliters of xylene in the reaction kettle, stir, heat and reflux for water separation and react for 6 hours, concentrate the reaction solution, reclaim the solvent for recycling, cool the reactant system, add water, separate out the solid product, wash and dry to obtain 39.9 grams of yellow Brown 1,4-bis(2,4-dinitrophenoxy)benzene crystal product with a purity of 99.5% and a melting point of 245°C, according to the actual obtained 1,4-bis(2,4-dinitrophenoxy) The amount of oxy)benzene and the theoretical amount (44.2 grams), the calculated yield of 1,4-bis(2,4-dinitrophenoxy)benzene was 90.2%.

Embodiment 3

[0033] 11.0 grams (0.10 moles) of hydroquinone, 40.5 grams (0.20 moles) of 2,4-dinitrochlorobenzene, 10.6 grams (0.10 moles) of sodium carbonate, 40 milliliters of N-methyl-2-pyrrolidone and 15 One milliliter of dichlorobenzene was put into the reaction kettle, stirred, heated to reflux and separated from water for 16 hours, concentrated the reaction solution, recovered the solvent for recycling, cooled the reactant system, added water, precipitated a solid product, washed and dried to obtain 41.2 g Yellow-brown 1,4-bis(2,4-dinitrophenoxy)benzene crystal product with a purity of 99.2%, according to the actual obtained 1,4-bis(2,4-dinitrophenoxy) The amount of benzene and the theoretical yield (44.2 g), the calculated yield of 1,4-bis(2,4-dinitrophenoxy)benzene was 93.2%.

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Abstract

The invention relates to a method for preparing 1- 4-bis(2-4-Nitrophenoxy) ethoxy benzene. The steps are as follows: (1) carrying out a heating reflux water division reaction for 6 to 18 hours on a p-dihydroxybenzene and a 2,4-dinitro halogenated benzene with a molar ratio of 1.0:2.0 to 2.2 in a system of salt forming agent and organic solvent; (2) concentrating a reaction fluid, cooling a reactant system, adding water to precipitate a solid product, fitering, washing and then drying to acquire the filemot 1 -4-bis(2-(4-Nitrophenoxy)ethoxy benzene. The invention has the advantages of simple operation, high yield and purity. Furthermore, the solvent is easy to be recovered and can be used repeatedly, which assures less waste gas, waste water and waste solid and is friendly to environmental and suitable for 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)benzene. 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)benzene 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. Aromatic polyval...

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