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Method for synthesizing 2-(5-fluoro-2, 4 dinitro-phenoxy) acetate

A technology for dinitrophenoxy and dinitrobenzene, which is applied in the field of synthesizing 2-acetate, can solve the problems of severe nitration reaction conditions, easy cleavage of ether bonds, low product yield and the like, and achieves rapid reaction and conversion rate. High, selective effect

Inactive Publication Date: 2019-05-14
内蒙古世杰化工有限公司
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  • Summary
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  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Among the various synthetic techniques that have been published so far, there are m-dichlorobenzene as raw materials, and the precursor 2-(5-fluoro-2,4-dinitrophenoxy) is obtained through nitration, fluorination, etherification and other steps. Acetate, when dichlorofluorinated to difluoro, the amount of tar is large, the product loss is large, etherification will produce impurities that both fluorines are etherified
There is 2,4-difluoronitrobenzene as the raw material, which undergoes hydrolysis, etherification, reduction, nitration, and reduction. Although the raw material is easy to obtain in this route, the route is long and the impurities are high. At the same time, hydrogenation is required twice, and the cost is increased. , cumbersome operation
There is m-fluorophenol as the starting material, although the reaction route is not very long, but the raw material is rare and expensive, the nitration reaction conditions are severe, the ether bond is easy to break, the impurities are high, and the product yield is low

Method used

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  • Method for synthesizing 2-(5-fluoro-2, 4 dinitro-phenoxy) acetate

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Embodiment Construction

[0020] The following will clearly and completely describe the technical solutions in the embodiments of the present invention with reference to the accompanying drawings in the embodiments of the present invention. Obviously, the described embodiments are only some, not all, embodiments of the present invention. Based on the embodiments of the present invention, all other embodiments obtained by persons of ordinary skill in the art without making creative efforts belong to the protection scope of the present invention.

[0021] see figure 1 , a method for synthesizing 2-(5-fluoro-2,4 dinitrophenoxy) acetate, using 2,4-dichloro-1,5-dinitrobenzene as raw material through hydrolysis, etherification, Fluorination reaction and work-up to obtain 2-(5 - Fluoro-2,4-dinitrophenoxy)acetate.

[0022] A further technical solution of the present invention comprises the following steps:

[0023] (1) Hydrolysis reaction

[0024] Put 175g of 30% liquid caustic soda into a 500ml reaction f...

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Abstract

The invention discloses a method for synthesizing 2-(5-fluoro-2, 4 dinitro-phenoxy) acetate. 2, 4-dichloro-1, 5-dinitrobenzene serves as a raw material, hydrolysis reaction of the 2, 4-dichloro-1, 5-dinitrobenzene and inorganic base is implemented to obtain 5-chlorine-2, 4-dinitrophenol salt, the 5-chlorine-2, 4-dinitrophenol salt is extracted by dichloroethane, etherification reaction of the 5-chlorine-2, 4-dinitrophenol salt and chloroacetate in aprotic solvent dichloroethane is implemented to obtain 2-(5-chlorine-2, 4-dinitro-phenoxy) acetate, and the 2-(5-chlorine-2, 4-dinitro-phenoxy) acetate and potassium fluoride are fluoridated to obtain 2-(5-fluorine-2, 4-dinitro-phenoxy) acetate. Reaction raw materials in all steps are easy to obtain and economical, technological conditions are mild, a line is short, operation is simple and convenient, the method is high in safety and short in reaction time, and industrial production can be popularized.

Description

technical field [0001] The invention relates to the technical field of herbicide production and preparation, in particular to a method for synthesizing 2-(5-fluoro-2,4-dinitrophenoxy) acetate. Background technique [0002] 2-(5-fluoro-2,4-dinitrophenoxy) acetate is a kind of pesticide intermediate, which can synthesize the herbicide flumechlor, which is protoporphyrinogen oxidase ( PPO) inhibitors are used to control weeds and broad-leaved weeds on soybeans, cotton, grapes and many other crops. The chemical structure of 2-(5-fluoro-2,4-dinitrophenoxy)acetate is as follows. Its chemical structural formula is as follows: [0003] [0004] Among the various synthetic techniques that have been published so far, there are m-dichlorobenzene as raw materials, and the precursor 2-(5-fluoro-2,4-dinitrophenoxy) is obtained through nitration, fluorination, etherification and other steps. When acetic ester is fluorinated from dichloro to difluoro, the amount of tar is large and the...

Claims

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Application Information

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IPC IPC(8): C07C201/12C07C205/26C07C205/37
Inventor 不公告发明人
Owner 内蒙古世杰化工有限公司
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