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Method for simply synthesizing pyraclostrobin

A pyraclostrobin, a concise technology, applied in the field of organic compound synthesis, can solve problems such as potential safety hazards, many reaction by-products, etc., and achieve the effects of promoting methylation speed, simplifying experimental conditions, and avoiding hydrolysis by-products

Active Publication Date: 2017-05-31
SICHUAN FOURSTAR BIOTECH RANDD CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] In order to provide a methylation synthesis process with simple operation, easy industrialization, fast and efficient reaction and low price, the present invention proposes a simple method for synthesizing pyraclostrobin, by rationally controlling the input sequence of reaction raw materials and system temperature , which effectively solves the problems of many reaction by-products and hidden safety hazards in the existing pyraclostrobin synthesis process, and can bring many benefits to industrial production such as reducing production costs and reducing the amount of waste water in the production process. conditions, making it beneficial for pesticide and chemical enterprises to save energy, reduce emissions and protect the environment, and more suitable for large-scale industrial production

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  • Method for simply synthesizing pyraclostrobin
  • Method for simply synthesizing pyraclostrobin
  • Method for simply synthesizing pyraclostrobin

Examples

Experimental program
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Effect test

Embodiment 1

[0044] This embodiment relates to a simple method for synthesizing pyraclostrobin, the content is as follows:

[0045] Put 330kg of pyraclostrobin intermediate and 8.25kg of phase transfer catalyst (benzyltriethylammonium chloride) into a 3000L reaction kettle, and then put 2310kg of organic solvent (methyl tert-butyl ether ) to dissolve, start stirring and freezing the saline solution to maintain the temperature of the system at 45°C, then put 121kg of dimethyl sulfate into the reactor, and add 350kg of 12% sodium hydroxide aqueous solution dropwise at this temperature, and the dropping time is controlled at After 60 minutes, after the dropwise addition was completed and incubated for 2 hours, samples were taken, and the reaction was stopped after HPLC monitoring until the peak area percentage of the pyraclostrobin intermediate was less than 0.5%.

[0046] After the reaction is completed, heat the steam to 60°C and keep it warm for 3 hours. After the heat preservation is comp...

Embodiment 2

[0049] This embodiment relates to a simple method for synthesizing pyraclostrobin, the content is as follows:

[0050] Put 350kg of pyraclostrobin intermediate and 7kg of phase transfer catalyst (benzyltriethylammonium chloride) into a 3000L reaction kettle, then put 2800kg of organic solvent (chloroform) from the storage tank to dissolve, and start stirring Keep the temperature of the system at 20°C with frozen saline solution, then put 130kg of dimethyl sulfate into the reaction kettle, and add 560kg of 8% sodium hydroxide aqueous solution dropwise at this temperature, the dropping time is controlled at 30 minutes, and the dropping is completed Samples were taken after incubation for 2 hours, and the reaction was stopped after HPLC monitoring until the peak area percentage of the pyraclostrobin intermediate was less than 0.5%.

[0051] After the reaction is completed, heat the steam to 65°C and keep it warm for 3 hours. After the heat preservation is completed, let it stand ...

Embodiment 3

[0054] This example relates to a method for concisely synthesizing pyraclostrobin, the content is as follows:

[0055] Put 365kg of pyraclostrobin intermediate and 16.5kg of phase transfer catalyst (tetraethylammonium bromide, tetrabutylammonium chloride and tetrabutylammonium bromide) into a 3000L reactor, and then from the storage tank Put 2920kg of organic solvent (dichloromethane) to dissolve, start stirring and freezing the saline solution to maintain the temperature of the system at 15°C, then put 135kg of dimethyl sulfate into the reaction kettle, and add 12% hydroxide dropwise at this temperature 390g of sodium aqueous solution, the dropping time is controlled at 50 minutes, after the dropping is completed and kept warm for 2 hours, the sample is taken, and the reaction is stopped after HPLC monitoring until the peak area percentage of the pyraclostrobin intermediate is less than 0.5%.

[0056] After the reaction is completed, heat the steam to 60°C and keep it warm fo...

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Abstract

The invention discloses a method for simply synthesizing pyraclostrobin. The method comprises steps as follows: N-hydroxyl-N-2-[1-(4-chlorophenyl)-3-pyrazoloxy methyl]phenyl carbamate and a phase transfer catalyst are dissolved in an organic solvent, dimethyl sulfate is added, an acid-binding agent is dropwise added at the system temperature kept in a range of 5-70 DEG C, the components react for 1-5 h, and pyraclostrobin is obtained. Under the condition of reasonable control of feeding sequence of reaction raw materials and the system temperature, the problems of many reaction by-products as well as potential safety hazard and the like due to the many reaction by-products in an existing pyraclostrobin synthesis process are effectively solved, and a plurality of advantages such as reduction of production cost, reduction of wastewater quantity in a production process and the like can be provided for industrial production, so that the method is beneficial to energy conservation, emission reduction and environment protection of pesticide chemical enterprises and is more suitable for large-scale industrial production.

Description

technical field [0001] The invention relates to a simple and efficient method for synthesizing pyraclostrobin, in particular to a simple and efficient industrial production method for synthesizing pyraclostrobin, which belongs to the field of organic compound synthesis. Background technique [0002] Pyraclostrobin (Pyraclostrobin) alias pyraclostrobin, chemical name: N -Methoxy- N -2-[1-(4-Chlorophenyl)-3-pyrazolyloxymethyl]phenylcarbamate is a high-efficiency product developed by BASF in 1993 and registered in 2001. It is a new methoxyacrylate fungicide with low toxicity and broad spectrum, and it is also the world's first fungicide product registered with "plant health effect". The fungicide is a mitochondrial respiration inhibitor, which can effectively prevent and treat crop diseases caused by Ascomycetes, Basidiomycetes, Oomycetes and Deuteromycetes, and is widely used in the prevention and treatment of rice, wheat, fruits and vegetables, and other field crops. disea...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D231/22
Inventor 刘虎王文李舟马青伟陈熙王蕾张华
Owner SICHUAN FOURSTAR BIOTECH RANDD CORP
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