Method for preparing 2,2-dual [3-amido-4-(4-nitrophenoxy)phenyl group]-1,1,1,3,3,3-hexa-fluoropropane

A technology of nitrophenoxy and hexafluoropropane is applied in the field of preparation of aromatic organic compounds and achieves the effects of less three wastes, less types of use and less investment

Inactive Publication Date: 2008-02-27
DONGHUA UNIV
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  • Abstract
  • Description
  • Claims
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AI Technical Summary

Problems solved by technology

[0026] But the preparation method of 2,2-bis[3-amino4-(4-nitrophenoxy)phenyl]-1

Method used

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  • Method for preparing 2,2-dual [3-amido-4-(4-nitrophenoxy)phenyl group]-1,1,1,3,3,3-hexa-fluoropropane
  • Method for preparing 2,2-dual [3-amido-4-(4-nitrophenoxy)phenyl group]-1,1,1,3,3,3-hexa-fluoropropane
  • Method for preparing 2,2-dual [3-amido-4-(4-nitrophenoxy)phenyl group]-1,1,1,3,3,3-hexa-fluoropropane

Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0051] Example 1

[0052] 36.6 g (0.10 mol) 2,2-bis(3-amino-4-hydroxyphenyl)-1,1,1,3,3,3-hexafluoropropane, 47.3 g (0.30 mol) 4-chloro Nitrobenzene, 110.4 g (0.80 mol) potassium carbonate, 700 ml of N,N-dimethylformamide and 180 ml of toluene were put into the reaction kettle, filled with nitrogen, stirred, heated to reflux and separated water to react for 18 hours, then concentrated for reaction Liquid, recover the solvent for recycling, cool the reactant system, add water, precipitate the solid product, wash, and dry to obtain 56.3 g of 2,2-bis[3-amino-4-(4-nitrophenoxy)phenyl] -1,1,1,3,3,3-hexafluoropropane with a purity of 99.0%. According to the actual situation, 2,2-bis[3-amino-4-(4-nitrophenoxy)phenyl]- The amount and theoretical amount of 1,1,1,3,3,3-hexafluoropropane (60.8 g), calculated to obtain 2,2-bis[3-amino-4-(4-nitrophenoxy)phenyl ] The yield of -1,1,1,3,3,3-hexafluoropropane was 92.6%.

Example Embodiment

[0053] Example 2

[0054] 36.6 g (0.10 mol) 2,2-bis(3-amino-4-hydroxyphenyl)-1,1,1,3,3,3-hexafluoropropane, 44.5 g (0.22 mol) 4-bromo Nitrobenzene, 55.2g (0.40mol) of potassium carbonate, 150ml of N,N-dimethylacetamide and 15ml of xylene were put into the reaction kettle, filled with nitrogen, stirred, heated to reflux and separated water to react for 4 hours, then concentrated The reaction liquid, the solvent is recovered for recycling, the reactant system is cooled, water is added, the solid product is precipitated, washed, and dried to obtain 27.7 g of 2,2-bis[3-amino-4-(4-nitrophenoxy)phenyl ]-1,1,1,3,3,3-hexafluoropropane with a purity of 98.9%. According to the actual situation, 2,2-bis[3-amino4-(4-nitrophenoxy)phenyl]- The amount and theoretical amount of 1,1,1,3,3,3-hexafluoropropane (60.8 g), calculated to obtain 2,2-bis[3-amino-4-(4-nitrophenoxy)phenyl ] The yield of -1,1,1,3,3,3-hexafluoropropane was 45.5%.

Example Embodiment

[0055] Example 3

[0056] 36.6 g (0.10 mol) 2,2-bis(3-amino-4-hydroxyphenyl)-1,1,1,3,3,3-hexafluoropropane, 31.5 g (0.20 mol) 4-chloro Nitrobenzene, 10.6 g (0.10 mol) of sodium carbonate, 40 ml of N-methyl-2-pyrrolidone and 15 ml of dichlorobenzene were put into the reaction kettle, filled with nitrogen, stirred, heated to reflux and separated water to react for 10 hours, The reaction solution was concentrated, the solvent was recovered for recycling, the reactant system was cooled, water was added, the solid product was precipitated, washed, and dried to obtain 47.5 g of 2,2-bis[3-amino-4-(4-nitrophenoxy)benzene Base]-1,1,1,3,3,3-hexafluoropropane, with a purity of 99.1%. According to the actual situation, 2,2-bis[3-amino-4-(4-nitrophenoxy)phenyl ]-1,1,1,3,3,3-hexafluoropropane amount and theoretical amount (60.8g), calculated to get 2,2-bis[3-amino-4-(4-nitrophenoxy) The yield of phenyl]-1,1,1,3,3,3-hexafluoropropane was 78.2%.

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Abstract

The invention discloses a making method of 2,2-di [3-amino-4-(4-nitrobenzeneoxy) phenyl]-1,1,1,3,3,3-hexafluoropropane, which comprises the following steps: (1) heating 2, 2-di (3-amino-4-hydroxybenzene)-1,1,1,3,3,3-hexafluoropropane and 4-halogenated nitrobenzene with molar rate at 1. 00: 2. 00-3. 00 under inert gas to reflux and do diversion reaction for 4-18h; (2) condensing the reacting liquid; cooling the reactant system; adding water; evolving solid product; filtering; washing; drying; obtaining the product. The invention simplifies the operation with high receiving rate and purity, which is easy to recycle solvent to use reciprocally to reduce three wastes for industrialized manufacturing.

Description

technical field [0001] The invention belongs to the field of preparation of aromatic organic compounds, in particular to a 2,2-bis[3-amino-4-(4-nitrophenoxy)phenyl]-1,1,1,3,3 , The preparation method of 3-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). Polyimide has many advantages as a liquid crystal aligning agent: [0003] (1) The coating itself has the function of aligning liquid crystal molecules; [0004] (2) It shows a good alignment ef...

Claims

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Application Information

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IPC IPC(8): C07C217/90C07C213/06
Inventor 虞鑫海
Owner DONGHUA UNIV
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