4,4-dinitrodiphenyl ethers synthesis method

A technology of dinitrodiphenyl ether and synthesis method, which is applied in 4 fields, can solve the problems of production equipment limitation, difficult industrial production, unfavorable production, etc., and achieve the effect of easy maintenance and use

Inactive Publication Date: 2006-04-26
EAST CHINA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The defect that the above-mentioned technology exists is that strong alkali is added in the initial reaction process, which means that the production equipment is greatly restricted. In addition...

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Add 31.5g p-nitrochlorobenzene, 7.6g sodium nitrite, 12g sodium bicarbonate, 100gDMF, 2g ethylene glycol in a 500ml three-necked flask equipped with a reflux condenser, a gas absorber, a thermometer and an electric stirrer, and heat Raise the temperature, the reaction temperature is 140°C, and maintain the reaction temperature for 3 hours, stop heating, wait to cool to room temperature, and filter with suction to obtain 4,4'-dinitrodiphenyl ether crystals, and the obtained product is washed with hot water at 95°C, Filter and dry in a vacuum oven (vacuum degree 0.06MPa, time 3h) to obtain 25.7g of dry crystalline product with a melting range of 142-143°C. Yield: 98.8%.

Embodiment 2

[0034] Add 31.5g p-nitrochlorobenzene, 7.6g sodium nitrite, 10g potassium bicarbonate, 100gDMA, 3g butanol in a 500ml three-necked flask equipped with a reflux condenser, a gas absorber, a thermometer and an electric stirrer, and heat up , the reaction temperature is 145°C, and keep the reaction temperature for 3.5h, stop heating, wait to cool to room temperature, and filter with suction to obtain 4,4'-dinitrodiphenyl ether crystals, the obtained product is washed with hot water at 95°C, Filter and dry in a vacuum oven (vacuum degree 0.06MPa, time 3h) to obtain 25.5g of dry crystalline product with a melting range of 142-143°C. Yield: 98.1%.

Embodiment 3

[0036] Add 31.5g p-nitrochlorobenzene, 7.6g sodium nitrite, 11g sodium carbonate, 100gDMSO, 2.5g butylene glycol in a 500ml three-necked flask equipped with a reflux condenser, a gas absorber, a thermometer and an electric stirrer, and heat Raise the temperature, the reaction temperature is 135°C, and maintain the reaction temperature for 3 hours, stop heating, wait to cool to room temperature, and filter with suction to obtain crystals of 4,4'-dinitrodiphenyl ether, wash the obtained product with hot water at 95°C, Filter and dry in a vacuum oven (vacuum degree 0.06MPa, time 3h) to obtain 24.5g of dry crystalline product with a melting range of 142-143°C. Yield: 94.2%.

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Abstract

The present invention discloses the synthesis of 4, 4'-dinitro diphenyl ether. The basic synthesis route is that under the action of proper catalyst and co-catalyst monobasic alcohol or polyhydric alcohol, the material p-nitrochlorobenzene is synthesized into 4, 4'-dinitro diphenyl ether. The synthesis process has yield up to 95 %, high reaction efficiency caused by the co-catalyst, no explosive side product and no corrosive material, and is suitable for industrial production.

Description

technical field [0001] The present invention relates to a kind of synthetic method of 4,4'-dinitrodiphenyl ether. Background technique [0002] 4,4'-Dinitrodiphenyl ether is an important intermediate in organic synthesis and polymer synthesis. In terms of organic synthesis, it can be used to replace carcinogenic benzidine to produce azo dyes and reactive dyes. Using it as a raw material, direct dyes with different color levels such as scarlet, bright red, sand red, yellow brown, green, gray, blue, bright orange, black, etc. have been developed, which can be used for dyeing silk wool, cotton, linen and other fabrics. Its color fastness and exhaustion rate are superior to benzidine dyes. In terms of polymer synthesis, the main use is to prepare 4,4'-diaminodiphenyl ether, which is a monomer for preparing high-temperature-resistant engineering plastic polyimide. It is also the raw material for the synthesis of 3,3',4,4'-tetraaminodiphenyl ether, which is used to prepare a se...

Claims

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Application Information

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IPC IPC(8): C07C205/38C07C201/12
Inventor 曹贵平张明华王凯云
Owner EAST CHINA UNIV OF SCI & TECH
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