Method for preparing 2,2-bi[3-amino-4-(2,6-dinitryl-4-trifluoromethyl phenoxy phenyl] propane

A technology of trifluoromethyl phenoxy and trifluoromethyl halogenated benzene is applied in the field of preparation of aromatic organic compounds, and achieves the effects of high product yield and purity, few types of use, and convenient recovery

Inactive Publication Date: 2009-04-08
DONGHUA UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] But the preparation method of 2,2-bis[3-amino-4-(2,6-dinitro-4-trifluoromethylphenoxy)phenyl]propane has no published patent or bibliographical information yet

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  • Method for preparing 2,2-bi[3-amino-4-(2,6-dinitryl-4-trifluoromethyl phenoxy phenyl] propane
  • Method for preparing 2,2-bi[3-amino-4-(2,6-dinitryl-4-trifluoromethyl phenoxy phenyl] propane

Examples

Experimental program
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Effect test

Embodiment 1

[0027] 25.8 grams (0.10 moles) of 2,2-bis(3-amino-4-hydroxyphenyl) propane, 59.5 grams (0.22 moles) of 2,6-dinitro-4-trifluoromethylchlorobenzene, 110.4 Gram (0.80 moles) salt of wormwood, 2064 milliliters of N, N-dimethylformamide and 207 milliliters of toluene are put into reaction kettle, stir, and under nitrogen atmosphere, after 18 hours of heating reflux water separation reaction, concentrate reaction solution, reclaim solvent To recycle, cool the reactant system, add water, precipitate a solid product, wash with hot water 2 to 3 times, and dry to obtain 68.2 grams of 2,2-bis[3-amino-4-(2,6-dinitro -4-trifluoromethylphenoxy)phenyl]propane crystal product with a purity of 99.6%, according to the actual acquisition of 2,2-bis[3-amino-4-(2,6-dinitro-4-tri The amount of fluoromethylphenoxy)phenyl]propane and the theoretical amount (72.6 g) was calculated to give 2,2-bis[3-amino-4-(2,6-dinitro-4-trifluoromethyl The yield of phenoxy)phenyl]propane was 94.0%.

Embodiment 2

[0029] 25.8 grams (0.10 moles) of 2,2-bis(3-amino-4-hydroxyphenyl) propane, 69.3 grams (0.22 moles) of 2,6-dinitro-4-trifluoromethylbromobenzene, 55.2 Gram (0.40 mole) potassium carbonate, 2000 milliliters of N, N-dimethylacetamide, 500 milliliters of benzene and 100 milliliters of dimethylbenzene are put into reaction kettle, stir, and under nitrogen atmosphere, after 15 hours of heating and reflux water separation reaction, concentrate Reaction solution, recovery solvent for recycling, cooling reactant system, adding water, precipitated solid product, washed 2 to 3 times with hot water, dried to obtain 70.0 g of 2,2-bis[3-amino-4-(2,6 -Dinitro-4-trifluoromethylphenoxy)phenyl]propane crystal product, the purity is 99.7%, according to the actual acquisition of 2,2-bis[3-amino-4-(2,6-dinitro - The amount of 4-trifluoromethylphenoxy)phenyl]propane and the theoretical amount (72.6 g) was calculated to give 2,2-bis[3-amino-4-(2,6-dinitro-4- The yield of trifluoromethylphenoxy)phe...

Embodiment 3

[0031] 25.8 grams (0.10 moles) of 2,2-bis(3-amino-4-hydroxyphenyl) propane, 54.1 grams (0.20 moles) of 2,6-dinitro-4-trifluoromethylchlorobenzene, 10.6 Gram (0.10 mole) sodium carbonate, 130 milliliters of N-methyl-2-pyrrolidone, 200 milliliters of benzene and 60 milliliters of dichlorobenzene are put into reaction kettle, stir, and under nitrogen atmosphere, after 12 hours of heating and reflux water separation reaction, Concentrate the reaction solution, recover the solvent for recycling, cool the reactant system, add water, and precipitate a solid product, wash with hot water 2 to 3 times, and dry to obtain 63.5 grams of 2,2-bis[3-amino-4-(2, 6-dinitro-4-trifluoromethylphenoxy)phenyl]propane crystal product, the purity is 99.2%, according to the 2,2-bis[3-amino-4-(2,6-di The amount of nitro-4-trifluoromethylphenoxy)phenyl]propane and the theoretical yield (72.6 g) were calculated to give 2,2-bis[3-amino-4-(2,6-dinitro- The yield of 4-trifluoromethylphenoxy)phenyl]propane w...

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Abstract

The invention relates to a method for preparing 2, 2-di [3-amino-4-(2, 6-dinitro-4-trifluoromethyl phenoxyl) phenyl] propane. The method comprises the following steps: (1) under nitrogen atmosphere, heating 2, 2-di (3-amino-4-hydroxyl phenyl) propane and 2, 6- dinitro-4-trifluoromethyl halogeno benzene with the molar ratio of 1.0 to 2.0-2.2, in a system of salifying agent and organic solvent, carrying out reflux and water separation reaction for 6 to 18 hours; and (2) condensing the reaction liquid, cooling the reactant system, adding water, separating out a solid product, filtering, washing and drying the solid product to obtain the 2, 2-di [3-amino-4-(2, 6-dinitro-4-trifluoromethyl phenoxyl) phenyl] propane. The method has the advantages of simple operation, high product yield and purity, convenient recovery for solvent, repeated use and few three wastes, is environment-friendly and suitable for industrial production.

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-(2,6-dinitro-4-trifluoromethylphenoxy)phenyl] Method for the preparation of 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-(2,6-dinitro-4-trifluoromethylphenoxy)phenyl]propane is a good choice for the synthesis of highly branched aromatic fluorine-containing polyimide monomers One of the ...

Claims

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Application Information

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IPC IPC(8): C07C217/90C07C213/06
CPCY02P20/582
Inventor 虞鑫海陈健丽刘斌陈梅芳
Owner DONGHUA UNIV
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