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Preparation method of 2,3-di(2,4-dinitro phenoxy)naphthalin

A technology of dinitrophenoxy and dinitro, which is applied in 2 fields to achieve the effects of convenient source, simple operation, high product yield and purity

Inactive Publication Date: 2008-10-15
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 2,3-bis(2,4-dinitrophenoxy)naphthalene has no disclosed patent or bibliographical information at present

Method used

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  • Preparation method of 2,3-di(2,4-dinitro phenoxy)naphthalin

Examples

Experimental program
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Effect test

Embodiment 1

[0026] 16.0 grams (0.10 moles) of 2,3-naphthalenediol, 44.6 grams (0.22 moles) of 2,4-dinitrochlorobenzene, 110.4 grams (0.80 moles) of potassium carbonate, 200 milliliters of N-methyl-2- Pyrrolidone, 500 milliliters of N, N-dimethylformamide and 180 milliliters of toluene were put into a reaction kettle, stirred, heated to reflux and separated from water for 18 hours, then concentrated the reaction liquid, recovered the solvent for recycling, cooled the reactant system, and added water , separate out the solid product, wash 2~3 times with hot water, dry, obtain 44.3 grams of 2,3-bis(2,4-dinitrophenoxy)naphthalene crystal product, the purity is 99.1%, according to the actual obtained 2 , 3-bis(2,4-dinitrophenoxy)naphthalene amount and theoretical amount (49.2 grams), calculate the yield of 2,3-bis(2,4-dinitrophenoxy)naphthalene was 90.1%.

Embodiment 2

[0028] 16.0 grams (0.10 moles) of 2,3-naphthalenediol, 54.4 grams (0.22 moles) of 2,4-dinitrobromobenzene, 55.2 grams (0.40 moles) of potassium carbonate, 150 milliliters of N-methyl-2- Pyrrolidone, 150 milliliters of N, N-dimethylacetamide, 100 milliliters of benzene and 15 milliliters of xylene were put into the reaction kettle, stirred, heated to reflux and separated from water for 6 hours, concentrated the reaction liquid, 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 38.8 grams of 2,3-bis(2,4-dinitrophenoxy)naphthalene crystal product with a purity of 99.5%. According to the actual amount of 2,3-bis(2,4-dinitrophenoxy)naphthalene and the theoretical amount (49.2 grams), 2,3-bis(2,4-dinitrophenoxy) was calculated The yield of naphthalene was 78.9%.

Embodiment 3

[0030] 16.0 grams (0.10 moles) of 2,3-naphthalenediol, 40.5 grams (0.20 moles) of 2,4-dinitrochlorobenzene, 10.6 grams (0.10 moles) of sodium carbonate, 180 milliliters of N-methyl-2- Pyrrolidone, 80 milliliters of benzene and 30 milliliters of dichlorobenzene were put into a 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, and precipitated a solid product. Wash 2~3 times with hot water, dry, obtain 34.5 grams of 2,3-bis(2,4-dinitrophenoxy)naphthalene crystal product, the purity is 99.1%, according to the actual obtained 2,3-bis( The amount of 2,4-dinitrophenoxy)naphthalene and the theoretical yield (49.2 g), the calculated yield of 2,3-bis(2,4-dinitrophenoxy)naphthalene was 70.2%.

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Abstract

The invention relates to a method for preparing 2,3-bis(2,4-dinitro phenoxyl) albocarbon. The method comprises the following steps: firstly, 2,3-dinitro halogeno benzene and 2,4-dinitro halogeno benzene in the mol ratio of 1.0:2.0-2.2 are subjected to heating reflux and water diversion reaction in a salt forming agent and an organic solvent system for 3 to 18 hours; secondly, the reacted liquor is concentrated, the reactant system is cooled down, water is added to separate the solid product out, filtering, cleaning and drying are performed to obtain the 2,3-bis(2,4-dinitro phenoxyl) albocarbon. The method has the advantages that the operation is simple, the product recovery rate and the purity are high, the solvent recovery is convenient, the solvent can be used repeatedly, the three wastes are less, the environment is not polluted, and the method is suitable for the industrialized production.

Description

technical field [0001] The invention belongs to the field of preparation of aromatic organic compounds, in particular to a preparation method of 2,3-bis(2,4-dinitrophenoxy)naphthalene. 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] 2,3-bis(2,4-dinitrophenoxy)naphthalene 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...

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
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