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Preparation method of 1-(4-chlorophenyl)-3-pyrazole alcohol

A technology of chlorophenyl and pyrazolidine, which is applied in the field of preparation of 1--3-pyrazolol, which can solve the problems of high temperature, large energy consumption, high cost of raw materials, etc.

Inactive Publication Date: 2016-10-12
SHANDONG EFIRM BIOCHEMISTRY & ENVIRONMENTAL PROTECTION CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The former DMF requires a higher temperature for desolvation under reduced pressure, and the energy consumption is large; the latter potassium hydroxide is relatively expensive, and the cost of raw materials is high

Method used

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  • Preparation method of 1-(4-chlorophenyl)-3-pyrazole alcohol
  • Preparation method of 1-(4-chlorophenyl)-3-pyrazole alcohol
  • Preparation method of 1-(4-chlorophenyl)-3-pyrazole alcohol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] First add 60g of acetic acid into the device, add 19.66g (0.1mol) of 1-(4-chlorophenyl)pyrazolidin-3-one and 0.0162g (0.0001mol) of ferric chloride under stirring, and heat up to 50°C , react with air, remove most of the solvent under reduced pressure after 4h, add water and stir, a large amount of product precipitates, adjust the pH value to 7 with sodium hydroxide solution, continue stirring for 0.5h, filter to obtain 1-(4-chlorophenyl)- 3-pyrazolol 19.4g, yield 99.7%, content 99.6% (LC).

Embodiment 2

[0023] First add 100g of 88% formic acid to the device, add 19.66g (0.1mol) of 1-(4-chlorophenyl)pyrazolidin-3-one and 1.62g (0.01mol) of ferric chloride under stirring, and heat up To 100°C, react with air, remove most of the solvent under reduced pressure after 4h, add water and stir, a large amount of product precipitates, adjust the pH value to 5 with sodium hydroxide solution, continue stirring for 0.5h, and filter to obtain 1-(4-chlorobenzene Base)-3-pyrazolol 19.32g, yield 99.3%, content 99.1% (LC).

Embodiment 3

[0025] First add 80g of propionic acid into the device, add 19.66g (0.1mol) of 1-(4-chlorophenyl)pyrazolidin-3-one and 0.81g (0.005mol) of ferric chloride under stirring, and heat up to 80 After 4 hours, remove most of the solvent under reduced pressure, add water and stir, a large amount of product precipitates, adjust the pH value to 8 with sodium hydroxide solution, continue stirring for 0.5h, and filter to obtain 1-(4-chlorophenyl) -3-pyrazolol 19.28g, yield 99.1%, content 99.7% (LC).

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Abstract

The invention relates to a preparation method of 1-(4-chlorophenyl)-3-pyrazolol, which belongs to the technical field of preparation of pesticide intermediates. Included steps: first acidic solvent is added in the device, under stirring, add 1-(4-chlorophenyl) pyrazolidin-3-ketone, iron trichloride, heat up to completely dissolve, ventilate and react, and the reaction ends Finally, remove most of the solvent under reduced pressure, add water and stir, and a large amount of products are precipitated. After adjusting the pH value with sodium hydroxide solution, continue stirring for 0.5h, and filter to obtain 1-(4-chlorophenyl)-3-pyrazolol. Advantages: the acidic solvent is cheap and easy to obtain, the reaction is homogeneous, the energy consumption of desolventization is low, the yield is high, the production cost is low, and it is suitable for industrial production.

Description

technical field [0001] The invention belongs to the technical field of preparation of pesticide intermediates, in particular to a preparation method of 1-(4-chlorophenyl)-3-pyrazolol. Background technique [0002] 1-(4-Chlorophenyl)-3-pyrazol is a key intermediate in the synthesis of methoxyacrylate fungicide pyraclostrobin. At present, according to literature reports, the synthesis of 1-(4-chlorophenyl)-3-pyrazolol is all obtained through oxidation reaction using 1-(4-chlorophenyl)pyrazolidin-3-one as raw material. The main difference in the process is the solvent, which is divided into DMF and 5% potassium hydroxide solution. The former DMF requires a higher temperature for desolvation under reduced pressure, and the energy consumption expenditure is large; the latter potassium hydroxide is relatively expensive, and the cost of raw materials is high. Contents of the invention [0003] The purpose of the present invention is to provide a kind of 1-(4-chlorophenyl)-3-pyr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D231/22
CPCC07D231/22
Inventor 于龙张超梁万根张宁闫敏敏
Owner SHANDONG EFIRM BIOCHEMISTRY & ENVIRONMENTAL PROTECTION CO LTD
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