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Preparation method for constructing compound with diphenyl ether structure

A technology of compound and diphenyl ether, which is applied in the field of preparation of diphenyl ether structure compounds, can solve the problems of difficult recycling of reaction solvents and catalysts, poisonous and harmful operators, long reaction time, etc., and achieves low cost of synthesis and preparation. The effect of good environment and easy operation

Active Publication Date: 2020-05-15
安徽禾宸化学科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there are still problems such as too long reaction time, difficult recycling of reaction solvent and catalyst, causing environmental pollution, and reaction solvent being poisonous and harmful to operators.

Method used

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  • Preparation method for constructing compound with diphenyl ether structure
  • Preparation method for constructing compound with diphenyl ether structure

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Preparation of compound 1

[0025] In the embodiment of the present invention, phenol is heated, a catalyst is added, and sodium hypochlorite solution is added dropwise. After the reaction is completed, the temperature is lowered, the reaction solution is acidified, ether is added for extraction, part of the ether is evaporated under reduced pressure, the temperature is lowered to crystallize, and the product is obtained after suction filtration and water washing. , specifically: use water as the reaction medium, adopt a one-pot method to synthesize diphenyl ether compounds, mix phenol and metal cuprous ion catalyst cuprous chloride into the reaction kettle by one-pot method, and add sodium hypochlorite aqueous solution dropwise at the same time to directly prepare diphenyl ether compounds. Phenyl ether structure compound, at first, sodium hypochlorite is uniformly dissolved in water, makes sodium hypochlorite aqueous solution, by weight, sodium hypochlorite: water=1: 10...

Embodiment 2

[0027] Preparation of compound 2

[0028] In the embodiment of the present invention, heat 2,6-dimethylphenol, add catalyst, dropwise add sodium hypochlorite solution, after the reaction, cool down, acidify the reaction solution, add solvent for extraction, separate layers, evaporate part of the solvent from the organic phase under reduced pressure , cooling and crystallization, and suction filtration to obtain the product after washing with water. Specifically, using water as the reaction medium, a diphenyl ether compound is synthesized by a one-pot method, and 2,6-dimethylphenol and the catalyst cuprous iodide are synthesized by a one-pot method Mix, add dropwise sodium hypochlorite aqueous solution, directly prepare diphenyl ether structure compound, at first, sodium hypochlorite is uniformly dissolved in water, obtain sodium hypochlorite aqueous solution, wherein by weight, sodium hypochlorite: water=1: 10; 2,6-dimethylphenol : catalyst cuprous iodide=10:1, in molar ratio,...

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Abstract

The invention discloses a preparation method for constructing a compound with a diphenyl ether structure, and belongs to the technical field of chemical engineering. The preparation method comprises following steps: adopting a one-pot method, reacting a raw material with sodium hypochlorite, a catalyst and phenol, heating, carrying out reflux reaction, regulating the pH value, carrying out solventextraction, carrying out reduced pressure distillation to remove the solvent, cooling , and precipitating to obtain the target product. The synthesis conditions are mild, water is used as a solvent,the target product is synthesized through a one-pot method, and the yield is high. Compared with the traditional Ullmann reaction, the provided preparation method only needs simple raw materials, theraw materials are abundant, the reaction temperature is low, and the product purity and yield are high. The preparation method can be used as a preferred method for synthesizing important medicine andpesticide products or organic intermediates, and has a wide industrial application prospect and practical value.

Description

technical field [0001] The invention belongs to the technical field of chemical industry, in particular to a preparation method for building diphenyl ether structure compounds. Background technique [0002] In 1904, Ullmann reported that halogenated aromatic hydrocarbons could react with metal salts of phenols to remove halogen salts to form corresponding diaryl hydrocarbon ethers. This reaction, known as the Ullmann reaction, is very common and can occur in water or polar media at elevated temperatures. The existing classic synthesis methods of diphenyl ether compounds are Ullmann method or Williamson method, the reaction conditions are harsh, difficult to control, and strict anhydrous is required. If an aprotic solvent (such as DMF, DMSO, etc.) is used, although the reaction conditions are mild, the solvent is expensive and difficult to recover. Sometimes it is necessary to add a small amount of catalyst such as potassium iodide, tetrabutylammonium bromide, etc. to promo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C41/01C07C43/23
CPCC07C41/01C07C43/23
Inventor 沈照亮陈博
Owner 安徽禾宸化学科技有限公司
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