Method for preparing 2,2-di[3-amino-4-(2,4-dinitrophenoxy)phenyl]hexafluoropropane

A technology of dinitrophenoxy and hexafluoropropane, applied in 2 fields, can solve problems such as patents or literature reports, and achieve the effects of fewer types of use, fewer three wastes, and convenient recovery

Inactive Publication Date: 2008-08-06
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] However, the preparation method of 2,2-bis[3-amino-4-(2,4-dinitrophenoxy)phenyl]hexafluoropropane has no published patent or bibliographical information yet.

Method used

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  • Method for preparing 2,2-di[3-amino-4-(2,4-dinitrophenoxy)phenyl]hexafluoropropane
  • Method for preparing 2,2-di[3-amino-4-(2,4-dinitrophenoxy)phenyl]hexafluoropropane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] 36.6 grams (0.10 moles) of 2,2-bis(3-amino-4-hydroxyphenyl) hexafluoropropane, 44.6 grams (0.22 moles) of 2,4-dinitrochlorobenzene, 110.4 grams (0.80 moles) Potassium carbonate, 700 milliliters of N,N-dimethylformamide and 180 milliliters of toluene were put into the reaction kettle, under nitrogen atmosphere, stirred, heated to reflux for water separation and reacted for 18 hours, concentrated the reaction solution, recovered the solvent for recycling, and cooled the reaction After 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]hexafluoro Propane, the purity is 99.1%, according to the actual amount and theoretical amount of 2,2-bis[3-amino-4-(2,4-dinitrophenoxy)phenyl]hexafluoropropane, 2 is calculated, The yield of 2-bis[3-amino-4-(2,4-dinitrophenoxy)phenyl]hexafluoropropane was 98.1%.

Embodiment 2

[0030] 36.6 grams (0.10 moles) of 2,2-bis(3-amino-4-hydroxyphenyl) hexafluoropropane, 54.4 grams (0.22 moles) of 2,4-dinitrobromobenzene, 55.2 grams (0.40 moles) Potassium carbonate, 150 milliliters of N, N-dimethylacetamide and 15 milliliters of dimethylbenzene 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, cooled The reactant system was added with water to precipitate a solid product, which was washed 2 to 3 times with hot water and dried to obtain 2,2-bis[3-amino-4-(2,4-dinitrophenoxy)phenyl]6 Fluoropropane, with a purity of 99.5%, is calculated based on the actual amount and theoretical amount of 2,2-bis[3-amino-4-(2,4-dinitrophenoxy)phenyl]hexafluoropropane. , the yield of 2-bis[3-amino-4-(2,4-dinitrophenoxy)phenyl]hexafluoropropane was 72.3%.

Embodiment 3

[0032] 36.6 grams (0.10 moles) of 2,2-bis(3-amino-4-hydroxyphenyl) hexafluoropropane, 40.5 grams (0.20 moles) of 2,4-dinitrochlorobenzene, 10.6 grams (0.10 moles) Sodium carbonate, 60 milliliters of N-methyl-2-pyrrolidone and 23 milliliters of dichlorobenzene were put into a reaction kettle, under a nitrogen atmosphere, stirred, heated to reflux for water separation and reacted for 16 hours, concentrated the reaction solution, recovered the solvent for recycling, Cool the reactant system, add water, precipitate a solid product, wash with hot water 2 to 3 times, and dry to obtain 2,2-bis[3-amino-4-(2,4-dinitrophenoxy)phenyl] Hexafluoropropane, with a purity of 99.2%, is calculated according to the amount and theoretical yield of 2,2-bis[3-amino-4-(2,4-dinitrophenoxy)phenyl]hexafluoropropane actually obtained The yield of 2,2-bis[3-amino-4-(2,4-dinitrophenoxy)phenyl]hexafluoropropane was 94.2%.

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Abstract

The invention relates to a preparation method of 2, 2-bis-[3-amino-4-(2, 4-dinitrophenoxy) phenyl] hexafluoropropane, comprising: (1) heating to reflux and segregate water for 6-18h to treat 2, 2-bis-(3-amino-4-hydroxy phenyl and 2, 4-dinitro halogenated benzene at a mol ratio of 1.0:2.0 to 2.2, in a system of salt forming agent and organic solvent, (2) concentrating reaction liquid, cooling the reactant system, adding water, precipitating solid product, filtering, washing and drying to obtain 2, 2-bis-[3-amino-4-(2, 4-dinitrophenoxy) phenyl] hexafluoropropane crystal. The preparation method of 2, 2-bis-[3-amino-4-(2, 4-dinitrophenoxy) phenyl] hexafluoropropane has simple operation, high yield and purity, wherein the solvent can be recovered easily and repeatedly used. The invention has low generation of three wastes and environment-friendly property, which is 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 2,2-bis[3-amino-4-(2,4-dinitrophenoxy)phenyl]hexafluoropropane. 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]hexafluoropropane is not only used for the synthesis of fluorine-containing polyimides and fluorine-containing polyimides containing strong polar nitro groups...

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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