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Method for preparing 2,2-di(3-amido-4-(2,4-dinitrophenoxy) phenyl] propane

A technology of dinitrophenoxy and dinitro, which is applied in 2 fields, can solve problems such as patents or literature reports, and achieve the effects of less types of use, simple operation, high yield and purity

Inactive Publication Date: 2008-07-30
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 2,2-bis[3-amino-4-(2,4-dinitrophenoxy group) phenyl]propane has no published patent or bibliographical information yet

Method used

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  • Method for preparing 2,2-di(3-amido-4-(2,4-dinitrophenoxy) phenyl] propane
  • Method for preparing 2,2-di(3-amido-4-(2,4-dinitrophenoxy) phenyl] propane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] 25.8 grams (0.10 moles) of 2,2-bis(3-amino-4-hydroxyphenyl) propane, 44.6 grams (0.22 moles) of 2,4-dinitrochlorobenzene, 110.4 grams (0.80 moles) of potassium carbonate , 70 milliliters of N,N-dimethylformamide and 280 milliliters of benzene were put into the reaction kettle, under nitrogen atmosphere, stirred, heated to reflux and separated from water for 18 hours, concentrated the reaction solution, recovered the solvent for recycling, and cooled the reactant system , add water, the solid product is separated out, washed 2 to 3 times with hot water, and dried to obtain 2,2-bis[3-amino-4-(2,4-dinitrophenoxy)phenyl]propane with a purity of 99.2%, according to the amount and theoretical amount of 2,2-bis[3-amino-4-(2,4-dinitrophenoxy)phenyl]propane actually obtained, the calculated 2,2-bis[3- The yield of amino-4-(2,4-dinitrophenoxy)phenyl]propane was 95.3%.

Embodiment 2

[0030] 25.8 grams (0.10 moles) of 2,2-bis(3-amino-4-hydroxyphenyl) propane, 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, 200 milliliters of benzene and 15 milliliters of xylene were put into the reaction kettle, under nitrogen atmosphere, stirred, heated to reflux and separated from water for 6 hours, concentrated the reaction solution, recovered the solvent for recycling , cooling the reactant system, adding water, the solid product was precipitated, washed 2 to 3 times with hot water, and dried to obtain 2,2-bis[3-amino-4-(2,4-dinitrophenoxy)phenyl ] propane, the purity is 99.5%, according to the actual amount and theoretical amount of 2,2-bis[3-amino-4-(2,4-dinitrophenoxy) phenyl] propane, calculate 2,2 - The yield of bis[3-amino-4-(2,4-dinitrophenoxy)phenyl]propane was 82.7%.

Embodiment 3

[0032] 25.8 grams (0.10 moles) of 2,2-bis(3-amino-4-hydroxyphenyl) propane, 40.5 grams (0.20 moles) of 2,4-dinitrochlorobenzene, 10.6 grams (0.10 moles) of sodium carbonate , 60 milliliters of N-methyl-2-pyrrolidone, 100 milliliters of benzene and 23 milliliters of dichlorobenzene were put into the reaction kettle, under a nitrogen atmosphere, stirred, heated to reflux for water separation and reacted for 16 hours, concentrated the reaction solution, and recovered the solvent for circulation Use, cool the reactant system, add water, precipitate a solid product, wash 2 to 3 times with hot water, and dry to obtain 2,2-bis[3-amino-4-(2,4-dinitrophenoxy)benzene Base] propane, the purity is 99.0%, according to the amount and theoretical yield of 2,2-bis[3-amino-4-(2,4-dinitrophenoxy)phenyl]propane actually obtained, calculate 2 , The yield of 2-bis[3-amino-4-(2,4-dinitrophenoxy)phenyl]propane was 95.1%.

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Abstract

The invention relates to a method for preparing 2, 2-double [3- amino-4-(2, 4- dinitrophenoxy) phenyl] propane, which comprises the steps that: (1) 2, 2-double(3- amino-4- hydroxyphenyl) propane 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 nitrogen atmosphere, 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 so as to precipitate the solid product; the obtained solutions are filtered and the obtained products are washed and dried so as obtain 2, 2-double [3- amino-4-(2, 4- dinitrophenoxy) phenyl] propane Crystal. 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 2,2-bis[3-amino-4-(2,4-dinitrophenoxy)phenyl]propane. 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] 2,2-bis[3-amino-4-(2,4-dinitrophenoxy)phenyl]propane is one of the important raw materials for the synthesis of aromatic polyimide monomers, that is, aromatic polybasic primary amines important raw materials. Ar...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C217/90C07C213/06C07C205/38C07C201/12
CPCY02P20/582
Inventor 虞鑫海
Owner DONGHUA UNIV
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