Preparation method of 2,2 bi-[3-nitryl-4-(2,6-dinitryl-4-trifluoromethyl phenoxy)phenyl] propane

A technology of trifluoromethylphenoxy and trifluoromethyl halogenated benzene is applied in the field of preparation of aromatic organic compounds and achieves the effects of less three wastes, convenient recovery and environmental friendliness

Inactive Publication Date: 2009-02-18
DONGHUA UNIV
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Problems solved by technology

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

Method used

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  • Preparation method of 2,2 bi-[3-nitryl-4-(2,6-dinitryl-4-trifluoromethyl phenoxy)phenyl] propane
  • Preparation method of 2,2 bi-[3-nitryl-4-(2,6-dinitryl-4-trifluoromethyl phenoxy)phenyl] propane

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Experimental program
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Effect test

Embodiment 1

[0028] 31.8 grams (0.10 moles) of 2,2-bis(3-nitro-4-hydroxyphenyl) propane, 59.5 grams (0.22 moles) of 2,6-dinitro-4-trifluoromethylchlorobenzene, 110.4 grams (0.80 moles) of potassium carbonate, 2544 milliliters of N, N-dimethylformamide and 260 milliliters of toluene were put into the reaction kettle, stirred, heated to reflux and separated from water for 18 hours, concentrated the reaction solution, recovered the solvent for recycling , cooling the reactant system, adding water, the solid product was precipitated, washed 2 to 3 times with hot water, and dried to obtain 72.3 grams of 2,2-bis[3-nitro-4-(2,6-dinitro-4 - Trifluoromethylphenoxy) phenyl] propane crystal product with a purity of 99.5%, according to the actual acquisition of 2,2-bis[3-nitro-4-(2,6-dinitro-4-trifluoro The amount of methylphenoxy)phenyl]propane and the theoretical amount (78.6 grams) was calculated to give 2,2-bis[3-nitro-4-(2,6-dinitro-4-trifluoromethyl The yield of phenoxy)phenyl]propane was 92.0%...

Embodiment 2

[0030] 31.8 grams (0.10 moles) of 2,2-bis(3-nitro-4-hydroxyphenyl) propane, 69.3 grams (0.22 moles) of 2,6-dinitro-4-trifluoromethyl bromobenzene, 55.2 grams (0.40 moles) of potassium carbonate, 1800 milliliters of N, N-dimethylacetamide, 250 milliliters of benzene and 150 milliliters of dimethylbenzene were put into a reaction kettle, stirred, heated to reflux and separated water for 12 hours, and concentrated 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 71.3 grams of 2,2-bis[3-nitro-4-(2,6-di Nitro-4-trifluoromethylphenoxy) phenyl] propane crystal product, the purity is 99.4%, according to the actual acquisition of 2,2-bis[3-nitro-4-(2,6-dinitro- The amount and theoretical amount of 4-trifluoromethylphenoxy)phenyl]propane (78.6 g) was calculated to give 2,2-bis[3-nitro-4-(2,6-dinitro-4- The yield of trifluoromethylphenoxy)phenyl]propane was ...

Embodiment 3

[0032] 31.8 grams (0.10 moles) of 2,2-bis(3-nitro-4-hydroxyphenyl) propane, 54.1 grams (0.20 moles) of 2,6-dinitro-4-trifluoromethylchlorobenzene, 10.6 grams (0.10 moles) of sodium carbonate, 160 milliliters of N-methyl-2-pyrrolidone, 280 milliliters of benzene and 40 milliliters of dichlorobenzene were put into the reaction kettle, stirred, heated to reflux and separated from water for 14 hours, and concentrated the reaction solution , 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 64.0 grams of 2,2-bis[3-nitro-4-(2,6- Dinitro-4-trifluoromethylphenoxy) phenyl] propane crystal product, the purity is 99.0%, according to the actual obtained 2,2-bis[3-nitro-4-(2,6-dinitro Base-4-trifluoromethylphenoxy)phenyl]propane amount and theoretical yield (78.6 g), calculated 2,2-bis[3-nitro-4-(2,6-dinitro- The yield of 4-trifluoromethylphenoxy)phenyl]propane was 81.4%.

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Abstract

The present invention relates to a preparation method of 2, 2-bis [3-nitro-4-(2, 6-dinitro-4-trifluoromethyl phenoxy) benzyl] propane. The preparation method comprises the following steps: firstly, 2, 2-bis (3-nitro-4-hydroxyphenyl) propane and 2, 6-dinitro-4-trifluoromethylphenyl halide with a molar ratio of from 1.0 to 2.0 to 2.2 are added into a system of salifying agent and organic solvent, and the system is heated and perform refluxing and water segregation reaction of 6 to 18 hours; secondly, the reaction solution is condensed, the reactant system is cooled, water is added, and solid products are separated, filtered, washed and dried to prepare the 2, 2-bis [3-nitro-4-(2, 6-dinitro-4-trifluoromethyl phenoxy) benzyl] propane. The present invention has the advantages that the operation is simple, the yield rate and purity of the product are high, the solvent recovery is convenient and the solvent can be repeatedly used, the three wastes are less, the preparation method is environment friendly, and the present invention is suitable for industrial production.

Description

technical field [0001] The invention belongs to the field of preparation of aromatic organic compounds, in particular to 2,2-bis[3-nitro-4-(2,6-dinitro-4-trifluoromethylphenoxy)phenyl ] Propane preparation method. 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-nitro-4-(2,6-dinitro-4-trifluoromethylphenoxy)phenyl]propane is a highly branched aromatic fluorine-containing polyimide monomer One of the important raw materials of aromatic fluorine-c...

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 虞鑫海徐永芬
Owner DONGHUA UNIV
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