Unlock instant, AI-driven research and patent intelligence for your innovation.

Preparation of 1,3,5-tri(2,6-dinitro- trifluoromethylphenoxy) benzene

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 yield and purity, few types of use and simple operation

Inactive Publication Date: 2008-10-08
DONGHUA UNIV +1
View PDF0 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] But the preparation method of 1,3,5-three (2,6-dinitro-4-trifluoromethylphenoxy) benzene, there is no published patent or literature report at present

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Preparation of 1,3,5-tri(2,6-dinitro- trifluoromethylphenoxy) benzene
  • Preparation of 1,3,5-tri(2,6-dinitro- trifluoromethylphenoxy) benzene

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] 12.6 grams (0.10 moles) of 1,3,5-pyrogallol, 86.6 grams (0.32 moles) of 2,6-dinitro-4-trifluoromethylchlorobenzene, 110.4 grams (0.80 moles) of potassium carbonate , 800 milliliters of N,N-dimethylformamide and 80 milliliters of benzene were put into the reaction kettle, stirred, heated to reflux and separated from water for 18 hours, concentrated the reaction liquid, recovered the solvent for recycling, cooled the reactant system, added water, Separate out solid product, wash 2~3 times with hot water, dry, obtain 80.6 grams of 1,3,5-three (2,6-dinitro-4-trifluoromethylphenoxy) benzene crystal product, purity It is 99.5%. According to the actual amount of 1,3,5-tri(2,6-dinitro-4-trifluoromethylphenoxy)benzene and the theoretical amount (82.8 grams), 1,3, The yield of 5-tris(2,6-dinitro-4-trifluoromethylphenoxy)benzene was 97.4%.

Embodiment 2

[0030] 12.6 grams (0.10 moles) of 1,3,5-pyrogallol, 100.8 grams (0.32 moles) of 2,6-dinitro-4-trifluoromethylbromobenzene, 55.2 grams (0.40 moles) of potassium carbonate , 700 milliliters of N, N-dimethylacetamide, 180 milliliters of benzene and 20 milliliters of xylene were put into the reaction kettle, stirred, and heated to reflux for water separation and reaction for 6 hours, then concentrated the reaction solution, recovered the solvent for recycling, and cooled the reaction After adding water, the solid product was separated out, washed 2 to 3 times with hot water, and dried to obtain 74.9 grams of 1,3,5-tris(2,6-dinitro-4-trifluoromethylphenoxy)benzene Crystalline product, the purity is 99.4%, according to the actual amount of 1,3,5-three (2,6-dinitro-4-trifluoromethylphenoxy) benzene obtained and the theoretical amount (82.8 grams), calculated The yield of 1,3,5-tris(2,6-dinitro-4-trifluoromethylphenoxy)benzene was 90.5%.

Embodiment 3

[0032] 12.6 grams (0.10 moles) of 1,3,5-pyrogallol, 81.2 grams (0.30 moles) of 2,6-dinitro-4-trifluoromethylchlorobenzene, 55.2 grams (0.40 moles) of potassium carbonate , 10.6 grams (0.10 moles) of sodium carbonate, 252 milliliters of N-methyl-2-pyrrolidone, 400 milliliters of benzene and 104 milliliters of dichlorobenzene were put into the reaction kettle, stirred, and heated to reflux for water separation for 16 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 76.6 grams of 1,3,5-tri(2,6-dinitro-4 -trifluoromethylphenoxy)benzene crystal product, the purity is 99.2%, according to the actual obtained 1,3,5-three (2,6-dinitro-4-trifluoromethylphenoxy)benzene Quantity and theoretical yield (82.8 g), the calculated yield of 1,3,5-tris(2,6-dinitro-4-trifluoromethylphenoxy)benzene was 92.5%.

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

The invention relates to a method to prepare 1,3,5-tri(2,6-binitro-4-trifluoromethyl-phenoxyl) benzene, including the following steps: (1), 1,3,5-phloroglucin and 2,6- binitro-4-trifluoromethyl-halogenated benzene based on molar ratio of 1.0:3.0-3.2 are heated to reflux and react for 6-18 hours in a system with salt forming agent and organic solvent;(2), the solution after reaction is concentrated and cooled, and then water is added to separate out the solid product, and after that the solution is filtrated, washed and dried, getting 1,3,5-tri(2,6-binitro-4-trifluoromethyl-phenoxyl)benzene crystalloid. The method is simple in operation with high yield and the product is high in purity; the solvent is convenient to recycle and can be used repeatedly; with little waste(gas, liquid and solid) and being environment-friendly, the method is applicable to industrial production.

Description

technical field [0001] The invention belongs to the field of preparation of aromatic organic compounds, in particular to a preparation method of 1,3,5-tris(2,6-dinitro-4-trifluoromethylphenoxy)benzene. 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] 1,3,5-tris(2,6-dinitro-4-trifluoromethylphenoxy)benzene is one of the important raw materials for the synthesis of highly branched aromatic polyimide monomers, that is, aromatic multi-primary An important raw ...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
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