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Method for preparing 2,7-di(2,4-dinitrophenoxy) naphthalene

A technology of dinitrophenoxy and dinitro, which is applied in 2 fields to achieve the effects of high product yield and purity, fewer types of use, and convenient recovery

Inactive Publication Date: 2008-07-30
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 2,7-bis(2,4-dinitrophenoxy)naphthalene, there is no published patent or literature report at present

Method used

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  • Method for preparing 2,7-di(2,4-dinitrophenoxy) naphthalene
  • Method for preparing 2,7-di(2,4-dinitrophenoxy) naphthalene
  • Method for preparing 2,7-di(2,4-dinitrophenoxy) naphthalene

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Experimental program
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Effect test

Embodiment 1

[0028] 16.0 grams (0.10 moles) of 2,7-naphthalenediol, 44.6 grams (0.22 moles) of 2,4-dinitrochlorobenzene, 110.4 grams (0.80 moles) of potassium carbonate, 700 milliliters of N,N-dimethyl Formamide and 180 milliliters of toluene were put into a reaction kettle, stirred, heated to reflux and separated from water for 18 hours, concentrated the reaction liquid, recovered the solvent for recycling, cooled the reactant system, added water, precipitated a solid product, washed, and dried to obtain 46.7 The 2,7-two (2,4-dinitrophenoxy) naphthalene crystal product of gram, purity is 99.6%, obtain 2,7-bis (2,4-dinitrophenoxy) naphthalene according to actual amount and theoretical amount (49.2 grams), the calculated yield of 2,7-bis(2,4-dinitrophenoxy)naphthalene is 95.1%.

Embodiment 2

[0030] 16.0 grams (0.10 moles) of 2,7-naphthalenediol, 54.4 grams (0.22 moles) of 2,4-dinitrobromobenzene, 55.2 grams (0.40 moles) of potassium carbonate, 150 milliliters of N,N-dimethyl Acetamide and 15 milliliters of xylene were put into a 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, added water, precipitated a solid product, washed, dried, and obtained 30.1 grams of 2,7-bis(2,4-dinitrophenoxy)naphthalene crystal product, the purity is 99.2%, according to the actual obtained 2,7-bis(2,4-dinitrophenoxy)naphthalene amount and theoretical amount (49.2 grams), the calculated yield of 2,7-bis(2,4-dinitrophenoxy)naphthalene is 61.3%.

Embodiment 3

[0032] 16.0 grams (0.10 moles) of 2,7-naphthalenediol, 40.5 grams (0.20 moles) of 2,4-dinitrochlorobenzene, 10.6 grams (0.10 moles) of sodium carbonate, 80 milliliters of N-methyl-2- Pyrrolidone and 30 milliliters of dichlorobenzene were 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, dried, Obtain 38.0 grams of 2,7-bis(2,4-dinitrophenoxy)naphthalene crystal product with a purity of 97.9%, according to the actual obtained 2,7-bis(2,4-dinitrophenoxy) The amount of naphthalene and the theoretical yield (49.2 g), the calculated yield of 2,7-bis(2,4-dinitrophenoxy)naphthalene was 77.2%.

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Abstract

The invention relates to a method for preparing 2, 7-double (-2, 4 dinitrophenoxy) naphthalene, which comprises the steps that: (1) 2, 7-naphthalenediol and 2, 4- dinitrohalobenzenes with a molar ratio ranging from 1.0 : 2.0 to 1.0 : 2.2 are subject to a heat refluxing and water diversion reaction for 6 to 18 hours in a system comprising the salt forming agents and organic solvents; (2) the reaction solution is concentrated, the reactant system is cooled and the water is added in the reactant system to precipitate the solid product; the obtained solutions are filtered, the obtained products are washed and dried so as to obtain 2, 4-double (-2, 4 dinitrophenoxy) naphthalene. The invention has simple operations and high product yield and purity, the solvents can be conveniently recycled and can be repeatedly used with few wastes, and the invention is environmentally friendly and suitable for 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 2,7-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] 2,7-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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Patent Type & Authority Applications(China)
IPC IPC(8): C07C205/38C07C201/12
CPCY02P20/582
Inventor 虞鑫海
Owner DONGHUA UNIV
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