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Production method of 4-(4-chlorophenoxy)-2-chloro phenyl-methyl ketone

A technology for the production of chlorophenoxy, which is applied in the field of intermediate synthesis of the agricultural fungicide oxafeconazole, can solve the problems of long reaction cycle and high efficiency, and achieve the effects of reducing production costs, reducing energy, and improving production efficiency

Inactive Publication Date: 2004-05-05
JIANGSU CHANGQING AGROCHEMICAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The synthesis of 4-(4-chlorophenoxy)-2-chlorophenyl-methyl ketone is disclosed in EP65485 GB2098607, but the yield is only about 60%, which needs to be improved; the reaction cycle is longer and requires more than 160°C reaction temperature

Method used

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  • Production method of 4-(4-chlorophenoxy)-2-chloro phenyl-methyl ketone
  • Production method of 4-(4-chlorophenoxy)-2-chloro phenyl-methyl ketone
  • Production method of 4-(4-chlorophenoxy)-2-chloro phenyl-methyl ketone

Examples

Experimental program
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Effect test

Embodiment 1

[0012] In a 250 ml reaction flask equipped with stirring, a thermometer, a reflux condenser and a dropping funnel, add 13.0 g (0.10 mole) of p-chlorophenol, 100 ml of xylene, and add 13.4 g (0.12 mole) of 50% potassium hydroxide aqueous solution dropwise at room temperature. ), after the dropwise addition, heat up and reflux to divide the water, and after the moisture is exhausted, decompress and go out xylene, drop into 80ml dimethyl sulfoxide in the dry p-chlorophenol salt that makes, 0.1g two (malate) copper ( II),

[0013]

[0014] Raise the temperature to 50°C, slowly add 19.2g (0.10mole) 2,4-dichloroacetophenone dropwise within 1.5 hours, then slowly raise the temperature to 100°C after the addition, and keep the reaction at this temperature for 3 hours, the reaction After the end, part of the DMSO was evaporated under negative pressure, and then quantitative toluene, water and dilute alkali solution were added, stirred, allowed to stand, and layered; the organic phas...

Embodiment 2

[0016] In a 250 ml reaction flask equipped with stirring, a thermometer, a reflux condenser and a dropping funnel, add 13.0 g (0.10 mole) of p-chlorophenol, 100 ml of xylene, and add 13.4 g (0.12 mole) of 50% potassium hydroxide aqueous solution dropwise at room temperature. ), after the dropwise addition, heat up and reflux to divide the water, after the moisture is exhausted, decompress and go out xylene, drop into 80ml dimethyl sulfoxide in the dry p-chlorophenate that makes, 0.5g two (malate) copper ( II),

[0017]

[0018] Raise the temperature to 50°C, slowly add 19.2g (0.10mole) 2,4-dichloroacetophenone dropwise within 1.5 hours, then slowly raise the temperature to 100°C after the addition, and keep the reaction at this temperature for 3 hours, the reaction After the end, part of the DMSO was evaporated under negative pressure, and then quantitative toluene, water and dilute alkali solution were added, stirred, allowed to stand, and layered; the organic phase was se...

Embodiment 3

[0020] In a 250 ml reaction flask equipped with stirring, a thermometer, a reflux condenser and a dropping funnel, add 13.0 g (0.10 mole) of p-chlorophenol, 100 ml of xylene, and add 13.4 g (0.12 mole) of 50% potassium hydroxide aqueous solution dropwise at room temperature. ), after the dropwise addition is completed, heat up and reflux to divide the water. After the moisture is exhausted, the dimethylbenzene is decompressed, and 80ml dimethyl sulfoxide, 0.1g bis(2-benzylaminopyridine) are dropped into the obtained dry p-chlorophenol salt ) copper(II),

[0021]

[0022] Raise the temperature to 50°C, slowly add 19.2g (0.10mole) 2,4-dichloroacetophenone dropwise within 1.5 hours, then slowly raise the temperature to 100°C after the addition, and keep the reaction at this temperature for 3 hours, the reaction After the end, part of the DMSO was evaporated under negative pressure, and then quantitative toluene, water and dilute alkali solution were added, stirred, allowed to ...

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Abstract

A process for preparing 4-(4-chlorophenoxy)-2-chlorophenyl-methylone as the intermediate of difenoconazole includes reacting between p-chlorophenol and 2,4-dichloro phenyl ethanone at 100 deg.C under catalysis of copper match, and separating. Its advantages are low reaction temp, and high output rate up to more than 95%.

Description

technical field [0001] The invention relates to an intermediate synthesis process of the agricultural fungicide oxafeconazole. Background technique [0002] 4-(4-Chlorophenoxy)-2-chlorophenyl-methyl ketone is an intermediate in the synthesis of the agricultural fungicide Difeconazole. Difeconazole is a triazole fungicide developed by Ciba Geigy AG. It has long-lasting protective and therapeutic activity against Ascomycetes, Basidiomycetes and Deuteromycetes, Erysidiomycetes, Rusts and certain species-borne diseases. The synthesis of 4-(4-chlorophenoxy)-2-chlorophenyl-methyl ketone is disclosed in EP65485 GB2098607, but the yield is only about 60%, which needs to be improved; the reaction cycle is longer and requires more than 160°C the reaction temperature. Contents of the invention [0003] The object of the present invention is to invent a kind of production method that improves reaction yield, reduces the new 4-(4-chlorophenoxy group)-2-chlorophenyl-methyl ketone of r...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/22C07C45/64C07C49/255
Inventor 吉志扬
Owner JIANGSU CHANGQING AGROCHEMICAL CO LTD
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