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Process for producing 4,4'bis(2,4-dinitrophenoxy) biphenyl

A technology of dinitrophenoxy and dinitro, applied in 4 fields, achieves the effects of high product yield and purity, few types of use, and convenient recovery

Inactive Publication Date: 2011-06-08
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] But the preparation method of 4,4'-bis(2,4-dinitrophenoxy)biphenyl has no disclosed patent or bibliographical information at present

Method used

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  • Process for producing 4,4'bis(2,4-dinitrophenoxy) biphenyl
  • Process for producing 4,4'bis(2,4-dinitrophenoxy) biphenyl
  • Process for producing 4,4'bis(2,4-dinitrophenoxy) biphenyl

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] 18.6 grams (0.10 moles) of 4,4'-diphenol, 44.6 grams (0.22 moles) of 2,4-dinitrochlorobenzene, 110.4 grams (0.80 moles) of potassium carbonate, 700 milliliters of N, N-di Methylformamide and 180 milliliters of toluene were put into the 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, dried, Obtain 50.3 grams of 4,4'-bis(2,4-dinitrophenoxy) biphenyl crystal product with a purity of 99.3%, according to the actual 4,4'-bis(2,4-dinitrobenzene The amount of oxy)biphenyl and the theoretical amount (51.8 grams), the calculated yield of 4,4'-bis(2,4-dinitrophenoxy)biphenyl is 97.1%.

Embodiment 2

[0029] 18.6 grams (0.10 moles) of 4,4'-diphenol, 54.4 grams (0.22 moles) of 2,4-dinitrobromobenzene, 55.2 grams (0.40 moles) of potassium carbonate, 150 milliliters of N, N-di Methyl acetamide and 15 ml 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, added water, precipitated a solid product, washed, and dried , Obtain 44.9 grams of 4,4'-bis(2,4-dinitrophenoxy) biphenyl crystal product, the purity is 98.7%, according to the actual obtained 4,4'-bis(2,4-dinitrobenzene The amount of oxy)biphenyl and the theoretical amount (51.8 grams), the calculated yield of 4,4'-bis(2,4-dinitrophenoxy)biphenyl was 86.7%.

Embodiment 3

[0031] 18.6 grams (0.10 moles) of 4,4'-diphenol, 40.5 grams (0.20 moles) of 2,4-dinitrochlorobenzene, 10.6 grams (0.10 moles) of sodium carbonate, 80 milliliters of N-methyl- Put 2-pyrrolidone and 30 ml of dichlorobenzene into the reaction kettle, stir, heat and reflux for water separation and react for 16 hours, concentrate the reaction solution, recover the solvent for recycling, cool the reactant system, add water, precipitate the solid product, wash, Dry to obtain 43.1 grams of 4,4'-bis(2,4-dinitrophenoxy) biphenyl crystal product with a purity of 99.0%. According to the actual obtained 4,4'-bis(2,4-dinitrophenoxy) According to the amount and theoretical yield (51.8 grams) of 4,4'-bis(2,4-dinitrophenoxy)biphenyl, the yield of 4,4'-bis(2,4-dinitrophenoxy)biphenyl was 83.3%.

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Abstract

The invention relates to a preparation method of 4,4'-double (2,4-dinitro phenoxy) biphenyl, which comprises the following steps: first the 4,4'-biphenyl diphenol and 2,4-dinitro halogenated benzene with the molar ratio of 1.0:2.0 to 2.2 are in heating refluxing water division reaction for 6 to 18 hours in a system of a salt forming agent and an organic solvent; second reaction solution is concentrated, reactant system is cooled, water is added, solid products is precipitated, filtered, washed and dried to obtain the 4,4'-double (2,4-dinitro phenoxy) biphenyl. The preparation method is characterized by simple operation, high product yield and purity, solvent being conveniently recovered and reused, little three waste, being environment friendly and being 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 4,4'-bis(2,4-dinitrophenoxy)biphenyl. 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] 4,4'-bis(2,4-dinitrophenoxy)biphenyl 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 pol...

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
Owner DONGHUA UNIV
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