Method for preparing 3,5-di(2,4-dinitro-phenoxy) benzoic acid

A technology of dinitrophenoxy and dihydroxybenzoic acid, applied in 3 fields, to achieve the effects of convenient source, high product yield and purity, and simple operation

Inactive Publication Date: 2008-07-23
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 3,5-bis(2,4-dinitrophenoxy)benzoic acid has no disclosed patent or bibliographical information at present

Method used

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  • Method for preparing 3,5-di(2,4-dinitro-phenoxy) benzoic acid
  • Method for preparing 3,5-di(2,4-dinitro-phenoxy) benzoic acid

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] 15.4 grams (0.10 moles) of 3,5-dihydroxybenzoic acid, 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 Put methyl formamide and 180 milliliters of toluene in the reaction kettle, stir, heat and reflux water separation reaction for 18 hours, concentrate the reaction solution, recover the solvent for recycling, cool the reactant system, add water, precipitate the solid product, wash and dry to obtain 46.3 grams of 3,5-bis(2,4-dinitrophenoxy)benzoic acid crystal product, the purity is 99.5%, according to the actual 3,5-bis(2,4-dinitrophenoxy) The amount of benzoic acid and the theoretical amount (48.6 grams), the calculated yield of 3,5-bis(2,4-dinitrophenoxy)benzoic acid is 95.2%.

Embodiment 2

[0028] 15.4 grams (0.10 moles) of 3,5-dihydroxybenzoic acid, 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 dimethylbenzene 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, added water, precipitated a solid product, washed, dried, Obtain 30.7 grams of 3,5-bis(2,4-dinitrophenoxy) benzoic acid crystal product with a purity of 99.0%, according to the actual 3,5-bis(2,4-dinitrophenoxy) The amount of benzoic acid and the theoretical amount (48.6 grams), the calculated yield of 3,5-bis(2,4-dinitrophenoxy)benzoic acid is 63.1%.

Embodiment 3

[0030] 15.4 grams (0.10 moles) of 3,5-dihydroxybenzoic acid, 40.5 grams (0.20 moles) of 2,4-dinitrochlorobenzene, 10.6 grams (0.10 moles) of sodium carbonate, 100 milliliters of N-methyl-2 - Pyrrolidone and 45 ml 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 solid product, washed and dried , to obtain 35.7 grams of 3,5-bis(2,4-dinitrophenoxy)benzoic acid crystal product with a purity of 96.1%. According to the actual obtained 3,5-bis(2,4-dinitrophenoxy Base) the amount of benzoic acid and the theoretical yield (48.6 grams), the calculated yield of 3,5-bis(2,4-dinitrophenoxy)benzoic acid is 73.5%.

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Abstract

The invention relates to a preparation method for 3,5-bis(2,4-dinitro phenoxy) benzoic acid, which comprises the following steps: (1) the 3,5-dihydroxybenzoic acid and 2,4-dinitro halogenated benzene with the molar ratio of 1.0: 2.0 to 2.2 are heated for refluence and water diversion reaction for 6 to 18 hours in the system of salt forming agent and organic solvent; (2) the reaction liquid is concentrated, the reactant system is cooled, water is added for precipitating the solid product, and the 3,5-bis(2,4-dinitro phenoxy) benzoic acid is gotten after filtering, washing and drying. The preparation method for 3,5-bis(2,4-dinitro phenoxy) benzoic acid has the advantages of simple operation, high product yield and purity, convenient solvent recovery, repeated use, less three wastes, environment-friendliness, and suitability for commercial production.

Description

technical field [0001] The invention belongs to the field of preparation of aromatic organic compounds, in particular to a preparation method of 3,5-bis(2,4-dinitrophenoxy)benzoic acid. 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] 3,5-bis(2,4-dinitrophenoxy)benzoic acid 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. Aromat...

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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