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Preparation method of 2,6-di(2,6-dinitro-4-trifluoromethyl phenoxy) benzotrifluoride

A technology of trifluoromethylphenoxy and hydroxytrifluorotoluene, which is applied in the field of preparation of aromatic organic compounds, and achieves the effects of fewer types of use, less waste, and convenient recycling

Inactive Publication Date: 2008-10-15
DONGHUA UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] But 2, the preparation method of 2,6-bis(2,6-dinitro-4-trifluoromethylphenoxy)benzotrifluoride does not have open patent or bibliographical information yet at present

Method used

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  • Preparation method of 2,6-di(2,6-dinitro-4-trifluoromethyl phenoxy) benzotrifluoride
  • Preparation method of 2,6-di(2,6-dinitro-4-trifluoromethyl phenoxy) benzotrifluoride

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Experimental program
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Effect test

Embodiment 1

[0027] 17.8 grams (0.10 moles) of 2,6-dihydroxybenzotrifluoride, 59.5 grams (0.22 moles) of 2,6-dinitro-4-trifluoromethylchlorobenzene, 110.4 grams (0.80 moles) of potassium carbonate, 1424 milliliters of N,N-dimethylformamide and 143 milliliters of benzene were put into the reaction kettle, stirred, heated to reflux and separated from water for 18 hours, then concentrated the reaction solution, recovered the solvent for recycling, cooled the reactant system, added water, and precipitated The solid product is washed 2 to 3 times with hot water and dried to obtain 63.6 grams of 2,6-bis(2,6-dinitro-4-trifluoromethylphenoxy)benzotrifluorotoluene crystal product with a purity of 99.5%, according to the actual amount of 2,6-bis(2,6-dinitro-4-trifluoromethylphenoxy)benzotrifluoride and the theoretical amount (64.6 grams), the calculated 2,6-bis The yield of (2,6-dinitro-4-trifluoromethylphenoxy)benzotrifluoride was 98.4%.

Embodiment 2

[0029] 17.8 grams (0.10 moles) of 2,6-dihydroxybenzotrifluoride, 69.3 grams (0.22 moles) of 2,6-dinitro-4-trifluoromethylbromobenzene, 55.2 grams (0.40 moles) of potassium carbonate, 800 milliliters of N, N-dimethylacetamide, 200 milliliters of N-methyl-2-pyrrolidone, 250 milliliters of benzene and 50 milliliters of xylene were put into the reaction kettle, stirred, heated to reflux and separated from water for 6 hours, then concentrated the reaction liquid, recover 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 53.4 grams of 2,6-bis(2,6-dinitro-4-tri Fluoromethylphenoxy)benzotrifluoride crystal product with a purity of 99.4%, according to the actual amount of 2,6-bis(2,6-dinitro-4-trifluoromethylphenoxy)benzotrifluoride obtained Based on the theoretical amount (64.6 g), the calculated yield of 2,6-bis(2,6-dinitro-4-trifluoromethylphenoxy)benzotrifluoride was 82.7%.

Embodiment 3

[0031] 17.8 grams (0.10 moles) of 2,6-dihydroxybenzotrifluoride, 54.1 grams (0.20 moles) of 2,6-dinitro-4-trifluoromethylchlorobenzene, 10.6 grams (0.10 moles) of sodium carbonate, Put 90 ml of N-methyl-2-pyrrolidone, 150 ml of benzene and 30 ml of dichlorobenzene into the reaction kettle, stir, heat to reflux and divide water for 12 hours, concentrate the reaction solution, recover the solvent for recycling, and cool the reaction After adding water, the solid product was precipitated, washed 2 to 3 times with hot water, and dried to obtain 51.9 grams of 2,6-bis(2,6-dinitro-4-trifluoromethylphenoxy)trifluorotoluene Crystalline product with a purity of 99.5%, based on the amount of 2,6-bis(2,6-dinitro-4-trifluoromethylphenoxy)benzotrifluoride actually obtained and the theoretical yield (64.6 grams), calculated The yield of 2,6-bis(2,6-dinitro-4-trifluoromethylphenoxy)benzotrifluoride was 80.4%.

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Abstract

The invention relates to a method for preparing 2,6-bis(2,6-binitro-4-trifluoromethylphenoxy pendant) benzotrifluoride, and comprises the following steps: firstly, 2,6-dihydroxytoluene and (2,6-binitro-4-trifluoromethylphenyl halides in the mol ratio of 1.0:2.0-2.2 are subjected to heating reflux and water diversion reaction in a salt forming agent and an organic solvent system for 6-18 hours; secondly, the reacted liquor is concentrated, the reactant system is cooled down, water is added to separate the solid product out, filtering, cleaning and drying are performed to obtain the 2,6-bis(2,6-binitro-4-trifluoromethylphenoxy pendant) benzotrifluoride. The method has the advantages that the operation is simple, the product recovery rate and the purity are high, the solvent recovery is convenient, the solvent can be used repeatedly, the three wastes are less, the environment is not polluted, and the method is suitable for the 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 2,6-bis(2,6-dinitro-4-trifluoromethylphenoxy)benzotrifluoride. 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] 2,6-bis(2,6-dinitro-4-trifluoromethylphenoxy)trifluorotoluene is one of the important raw materials for the synthesis of highly branched aromatic polyimide monomers, that is, aromatic multi-primary An im...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C205/38C07C201/12
CPCY02P20/582
Inventor 虞鑫海陈梅芳陈健丽刘斌
Owner DONGHUA UNIV
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