Preparation method of 2,5-bi(2-trifluoromethyl-4-aminophenoxyl)toluene

A technology of aminophenoxy and trifluoromethyl, which is applied in the field of preparation of aromatic fluorine-containing organic compounds, and achieves the effect of convenient source of raw materials, simple operation, and fewer types of use

Inactive Publication Date: 2013-06-26
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0011] 2,5-bis(2-trifluoromethyl-4-aminophenoxy)toluene is one of the important raw materials for the synthesis of aromatic fluorine-containing polyimide polymer materials, and there is no published patent literature report so far

Method used

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  • Preparation method of 2,5-bi(2-trifluoromethyl-4-aminophenoxyl)toluene
  • Preparation method of 2,5-bi(2-trifluoromethyl-4-aminophenoxyl)toluene
  • Preparation method of 2,5-bi(2-trifluoromethyl-4-aminophenoxyl)toluene

Examples

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Embodiment 1

[0033] With 47.4 grams (0.10 mole) 2,5-bis(2-trifluoromethyl-4-nitrophenoxy) toluene, 710 milliliters of ethanol solvent, 2.8 grams of palladium / carbon (the mass percent of metal palladium is 10 %) catalyst into the reactor, heating, stirring, heating up to 70 ℃ ~ 80 ℃, dropwise adding 112.6 grams of hydrazine hydrate aqueous solution with a mass percentage concentration of 80%, the dropping time is strictly controlled at 1-1.5 hours, after the dropping is completed , keep the reaction at 70℃~80℃ for 3 hours, filter while it is hot, remove the filter residue, keep the mother liquor, and add 500ml of deionized water dropwise to the mother liquor while stirring, let it stand for 8 hours, and precipitate a white solid product , filtered, washed 2-3 times with deionized water, and dried to obtain 40.5 grams of 2,5-bis(2-trifluoromethyl-4-aminophenoxy)toluene solid (theoretical yield: 41.4 grams), melting point 83.1 ℃ (DSC method, nitrogen atmosphere, heating rate 10 ℃ / min), purity...

Embodiment 2

[0037] 47.4 grams (0.10 moles) of 2,5-bis(2-trifluoromethyl-4-nitrophenoxy) toluene, 74 milliliters of ethylene glycol and 400 milliliters of ethanol solvent, 4.7 grams of palladium / carbon (the mass of metal palladium The percentage content is 1%) catalyst is added in the reactor, heating, stirring, heating up to 70 ℃~80 ℃, dropwise adding 117.7 grams of hydrazine hydrate aqueous solution with a mass percentage concentration of 85%, and the dropping time is strictly controlled within 1-1.5 hours After the dropwise addition is completed, keep the reaction at a temperature of 70°C to 80°C for 4 hours, filter while it is hot, remove the filter residue, keep the mother liquor, and add 474 ml of deionized water dropwise to the mother liquor while stirring, and let it stand for 5 hours , precipitated a white solid product, filtered, washed 2-3 times with deionized water, and dried to obtain 38.1 grams of 2,5-bis(2-trifluoromethyl-4-aminophenoxy)toluene solid (theoretical yield: 41.4 ...

Embodiment 3

[0039]With 47.4 grams (0.10 moles) 2,5-bis(2-trifluoromethyl-4-nitrophenoxy) toluene, 600 milliliters of ethanol solvent, 3.0 grams of palladium / carbon (the mass percent of metal palladium is 10 %) catalyst into the reactor, heating, stirring, heating up to 70 ℃ ~ 80 ℃, dropwise adding 58.9 grams of hydrazine hydrate aqueous solution with a mass percentage concentration of 85%, and the dropping time is strictly controlled at 1-1.5 hours. , keep the reaction at 70°C to 80°C for 2 hours, filter while it is hot, remove the filter residue, keep the mother liquor, add 300ml of deionized water dropwise to the mother liquor while stirring, let it stand for 6 hours, and precipitate a white solid product , filtered, washed 2-3 times with deionized water, and dried to obtain 39.7 grams of 2,5-bis(2-trifluoromethyl-4-aminophenoxy)toluene solid (theoretical yield: 41.4 grams), purity 99.7 %, product yield 96%.

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Abstract

The invention relates to a preparation method of 2,5-bi(2-trifluoromethyl-4-aminophenoxyl)toluene, comprising the steps of adding 2,5-bi(2-trifluoromethyl-4-nitrophenoxyl)toluene, an organic solvent, and a palladium / carbon catalyst in a reaction kettle, heating the reaction kettle, stirring, raising temperature to 70-80 DEG C, dripping a hydrazine hydrate aqueous solution, strictly controlling thedripping time within 1-1.5 hours, reacting for 2-4 hours at 70-80 DEG C after finishing dripping the aqueous solution, filtering when the solution is hot, removing filter residues, maintaining the mother liquid, dripping deionised water into the mother liquid while stirring, putting the mother liquid aside for 5-8 hours, separating out white solid product, filtering, washing and drying to obtain2,5-bi(2-trifluoromethyl-4-aminophenoxyl)toluene solid. The method has a simple technology, low cost, high purity and yield, and is environment-friendly and suitable for commercial production.

Description

technical field [0001] The invention belongs to the field of preparation of aromatic fluorine-containing organic compounds, in particular to a preparation method of 2,5-bis(2-trifluoromethyl-4-aminophenoxy)toluene. Background technique [0002] Aromatic polyimide has excellent thermal stability, chemical stability, 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] Fluorine-containing polyimide materials not only have the above-mentioned excellent properties, but also have very excellent optical transparency, flame retardancy and excellent molding processability. In addition, its dielectri...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C217/90C07C213/02
Inventor 虞鑫海张丽娟
Owner DONGHUA UNIV
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