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Synthetic method of pyraclostrobin intermediate pyrazole alcohol

A technology of pyraclostrobin and pyraclostrobin, which is applied in the synthesis process field of pyraclostrobin intermediate pyraclostrobin, can solve the problems of unfavorable economy, unfavorable economy, low yield, etc., and achieve Effects of optimizing synthesis process design, improving economic benefits, and saving synthesis costs

Inactive Publication Date: 2017-07-14
ANHUI GUANGXIN AGROCHEM
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Problems solved by technology

[0006] 1. There is no agitator or unreasonable setting of agitation parameters inside the oxidation reactor, which makes the synthesis efficiency and yield of pyraclostrobin intermediate pyraclostrobin low, which is not conducive to large-scale production;
[0007] 2. The organic liquid after desolventization has not been washed, resulting in DMF impurities in the final product, affecting the purity and actual use value of the product, which is not conducive to economy, and does not meet the actual requirements of green environmental protection and safety;
[0008] 3. The DMF recovered by precipitating is directly used in the oxidation reactor for reaction without purification, and new impurities are introduced. The liquid phase obtained after centrifugation is applied in the oxidation reactor for reproduction, which wastes the production cost. uneconomical

Method used

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  • Synthetic method of pyraclostrobin intermediate pyrazole alcohol

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Embodiment 1

[0028] see figure 1 As shown, the technical scheme adopted in the present invention is: a kind of synthesis process of pyraclostrobin intermediate pyrazol, and the specific process method includes the following steps:

[0029] (1). Oxidation: Put 1-(4-chlorophenyl)pyrazolidin-3-one into the oxidation reaction kettle, add the solvent DMF from the top side of the oxidation reaction kettle, and continue to pass through the top side of the oxidation reaction kettle. Enter oxygen for a period of time, use a stirrer to stir, keep warm in the oxidation reaction kettle for 1 hour, and transfer to the precipitation kettle after the oxidation reaction is completed;

[0030] (2). Precipitation: transfer the organic solution in the oxidation reaction kettle containing DMF into the precipitation kettle, use a stirrer to stir in the precipitation kettle, heat and evaporate the DMF, and transfer the DMF that evaporates to form steam into the solvent The recovery tower is used for recovery, ...

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Abstract

The invention discloses a synthetic method of a pyraclostrobin intermediate pyrazole alcohol. The process method specifically comprises the following steps: inputting 1-(4-chlorphenyl)-pyrazolidine-3-one in a reaction kettle; adding a solvent DMF and introducing oxygen for 5-6 hours; keeping the temperature for 1 hour; after oxidizing reaction, transferring the solution into a desolventizing kettle; evaporating and recovering DMF; after desolventization, adding water to wash and centrifugalize; and obtaining a solid phase light yellow solid 1-(4-chlorphenyl)-3-pyrazole. The synthetic method can effectively recover the solvent after initial reaction of the pyraclostrobin intermediate pyrazole alcohol, so that the synthetic cost is lowered, the economical benefit is improved, the synthetic process design of the pyraclostrobin intermediate pyrazole alcohol is optimized, and the demand on the synthetic process design of the pyraclostrobin intermediate pyrazole alcohol is met.

Description

technical field [0001] The invention relates to the technical field of pesticide synthesis, in particular to a synthesis process of pyraclostrobin intermediate pyraclostrobin. Background technique [0002] Methoxyacrylate fungicides are a class of low-toxicity, high-efficiency, broad-spectrum, systemic fungicides. They are new fungicides with great development potential and market vitality in the world’s pesticide industry; pyraclostrobin is currently the most active fungicide. A good methoxyacrylate fungicide, which was first developed and researched by BASF in Germany, and was launched in the European market in 2002; pyraclostrobin has the disadvantages of high efficiency, low toxicity, environmental friendliness, and a wide range of crops ; In the short few years since pyraclostrobin was listed, 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 a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D231/22
CPCC07D231/22
Inventor 黄金祥吴建平刘长庆戴玉婷黄显超杨亚明张军徐小兵朱张
Owner ANHUI GUANGXIN AGROCHEM
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