Process for synthesizing pyraclostrobin intermediate alpha-bromo-2-nitrotoluene

A technology of pyraclostrobin and nitrobenzyl bromide, which is applied in the synthesis process field of pyraclostrobin intermediate o-nitrobenzyl bromide, can solve the problems of unfavorable economy, low synthesis efficiency of o-nitrobenzyl bromide, Low yield and other problems, to achieve the effect of meeting the design of the synthesis process, optimizing the design of the synthesis process, and saving the cost of synthesis

CN107098812AInactive Publication Date: 2017-08-29ANHUI GUANGXIN AGROCHEM
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Patent Information

Authority / Receiving Office
CN · China
Current Assignee / Owner
Publication Date
2017-08-29
Estimated Expiration
Not applicable · inactive patent

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Abstract

The invention discloses a process for synthesizing a pyraclostrobin intermediate alpha-bromo-2-nitrotoluene. The process method specifically comprises the following steps: adding quantitative chlorobenzene and an HBr aqueous solution into the reactor, raising the temperature to be 40-50 DEG C, simultaneously dropwise adding ortho-nitrotoluene and hydrogen peroxide, and maintaining the temperature for 5-6 hours; transferring into a pH value regulation kettle after the reaction is ended, adding sodium hydroxide to regulate the pH value to be neutral; and transferring into an extraction kettle, standing and layering, extracting the organic phase, thereby obtaining the alpha-bromo-2-nitrotoluene chlorobenzene solution. According to the process disclosed by the invention, the solvent can be effectively recovered from the pyraclostrobin intermediate alpha-bromo-2-nitrotoluene after the primary reaction is ended, the synthetic cost is saved, the economic benefits are improved, the synthetic process design of the pyraclostrobin intermediate alpha-bromo-2-nitrotoluene is optimized, and the requirement on the synthetic process design of the pyraclostrobin intermediate alpha-bromo-2-nitrotoluene is met.
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Description

technical field

[0001] The invention relates to the technical field of pesticide synthesis, in particular to a synthesis process of pyraclostrobin intermediate o-nitrobenzyl bromide. 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 on...

Examples

Embodiment 1

[0026] see figure 1 Shown, the technical scheme that the present invention adopts is: a kind of synthetic technique of pyraclostrobin intermediate o-nitrobenzyl bromide, and the concrete of described process method comprises the following steps:

[0027] (1). Raw material measurement: Use the raw material metering tank to measure quantitative chlorobenzene and HBr aqueous solution, and transfer the quantitative chlorobenzene and HBr aqueous solution to the interior of the o-nitrobenzyl bromide synthesis kettle for reaction;

[0028] (2). Oxidative synthesis: After setting the temperature rise parameters and stirring parameters in the o-nitrobenzyl bromide synthesis kettle, add o-nitrotoluene and hydrogen peroxide dropwise into the o-nitrobenzyl bromide synthesis kettle, turn on the stirrer to stir and keep warm for a period of time time;

[0029] (3).PH value adjustment: After the reaction inside the o-nitrobenzyl bromide synthesis kettle is completed, transfer the bottom mat...