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Synthesis technology of pyraclostrobin

A pyraclostrobin and synthesis process technology, which is applied in the field of pyraclostrobin synthesis process, can solve the problems of unsuitability for industrial production, high cost of raw materials, low yield, etc., and achieve high catalytic efficiency and selectivity, Effects of improving yield and purity, and improving selective reducibility

Inactive Publication Date: 2016-10-12
ANHUI GUANGXIN AGROCHEM
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there is an ammonium chloride-zinc powder reduction method for the reduction reaction of o-nitrotoluene. The raw material price of this method is cheap, the cost is low, and it is safe and feasible, but the yield is usually not high, generally only reaching 50%-70%; Catalytic hydrogenation reduction method, using palladium or platinum as a catalyst, the method has high conversion rate and selectivity, but the raw material cost is expensive, and is not suitable for industrial production; Rh-hydrazine hydrate system reduces o-nitrotoluene, Rh is also expensive, and is not suitable for industrial production production, while the product yield can only reach about 70%

Method used

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  • Synthesis technology of pyraclostrobin
  • Synthesis technology of pyraclostrobin

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Embodiment 1

[0020] A kind of synthetic technique of pyraclostrobin mainly comprises the following steps:

[0021] (1) Under the catalysis of 0.4mol zinc powder and its alloy micronano powder, 0.2mol o-nitrotoluene and 0.2mol NH 4 Cl aqueous solution undergoes a reduction reaction, and the reaction temperature is controlled at 60°C, and then 0.04mol of n-propylamine is added. After the reaction is complete, excess zinc powder is filtered, and the filtrate is extracted with ethyl acetate, washed with water and dried, and then collected by desolvation under reduced pressure. The orange material is N-(2-methylphenyl)hydroxylamine;

[0022] (2) Add 0.2mol N-(2-methylphenyl) hydroxylamine, 0.4mol NaHCO in the reactor 3 and dichloromethane solvent, slowly drop 0.2mol of methyl chloroformate at a temperature of 3°C, keep warm after the dropwise addition, filter, wash with water, dry, and crystallize after reduced pressure distillation, the white solid obtained is N -Methyl hydroxy-N-2-tolueneca...

Embodiment 2

[0028] A kind of synthetic technique of pyraclostrobin mainly comprises the following steps:

[0029] (1) Under the catalysis of 0.6mol zinc powder and its alloy micronano powder, 0.3mol o-nitrotoluene and 0.3mol NH 4 A reduction reaction occurs in the aqueous Cl solution, the reaction temperature is controlled at 55°C, and 0.06mol of n-propylamine is added. After the reaction is complete, the filtrate is extracted with ethyl acetate, washed with water and dried, and the orange material obtained by desolvation under reduced pressure is N-(2-methylphenyl)hydroxylamine;

[0030] (2) Add 0.2mol of N-(2-methylphenyl) hydroxylamine, 0.4mol of NaHCO in the reactor 3 and dichloromethane solvent, slowly drop 0.26mol of methyl chloroformate at a temperature of 8°C, keep warm after the dropwise addition is completed, filter, wash with water, dry, and crystallize after reduced pressure distillation, the white solid obtained is N -Methyl hydroxy-N-2-toluenecarbamate;

[0031] (3) Add 0...

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Abstract

The invention provides a synthesis process of pyraclostrobin, which can be divided into five steps: (1) o-nitrotoluene and NH 4 Cl reduction reaction occurs under the catalysis of zinc powder and alloy micronano powder; (2) acylation reaction of hydroxylamine; (3) methylation reaction; (4) N-methoxy-N -2-bromomethylphenyl methyl carbamate; (5) use DMF as a solvent to dissolve N-methoxy-N-2-bromomethyl phenyl methyl carbamate and make a solution for subsequent use, and 1-( 4‑chlorophenyl)‑pyrazolol, K 2 CO 3 , acetone and put them into the reactor together, after heating up and refluxing, slowly add N-methoxy-N-2-bromomethylphenyl carbamate solution in the reactor, and the product pyrazole ether is obtained after the reflux reaction is completed Strostrobin. Compared with the prior art, the preparation method of the present invention is simple, the raw materials are cheap and easy to obtain, the reaction conditions are mild, and the purity and yield of the obtained target product are high.

Description

Technical field: [0001] The invention relates to a synthesis process of pyraclostrobin, in particular to the field of pesticide synthesis. Background technique: [0002] Methoxyacrylate fungicides are a class of low-toxicity, high-efficiency, broad-spectrum, systemic fungicides, and are new types of fungicides with great development potential and market vitality in the world's pesticide industry. Pyraclostrobin is currently the most active methoxyacrylate fungicide. It was first developed and researched by BASF in Germany and launched in the European market in 2002. Pyraclostrobin has the disadvantages of high efficiency, low toxicity, environmental friendliness, and wide application of crops. In just a few years since pyraclostrobin came into the market, the market of this variety has soared rapidly, and the sales have risen rapidly, and it has been listed as the second place in the market of all bacterial agents, second only to azoxystrobin. [0003] At present, there ar...

Claims

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Application Information

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IPC IPC(8): C07D231/22
CPCC07D231/22
Inventor 黄金祥过学军吴建平胡明宏杨亚明程伟家李红卫徐小兵黄显超戴玉婷
Owner ANHUI GUANGXIN AGROCHEM
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