Synthetic method of 2-methyl-4-chlorophenoxyacetic acid

A technology of o-methylphenoxyacetic acid and chlorophenoxyacetic acid is applied in chemical instruments and methods, separation/purification of carboxylic acid compounds, preparation of carboxylate salts, etc. phenol wastewater, incomplete neutralization and other problems, to achieve the effect of reducing energy consumption, improving production economy, and reducing by-products

Inactive Publication Date: 2015-09-30
ANHUI HUAXING CHEM IND CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Therefore, the global research on 2-methyl-4-chlorophenoxyacetic acid has not stopped so far.
[0003] The synthetic route of 2-methyl-4-chlorophenoxyacetic acid mainly adopts neutralization-condensation-chlorination, and most manufacturers use sodium hydroxide to neutralize and chlorine to chlorinate, but there is no neutralization in sodium hydroxide. The shortcomings of thoroughness and few by-products reduce the content and yield of the product; and the use of chlorine chlorination will produce a large amount of difficult-to-treat phenol-containing wastewater

Method used

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  • Synthetic method of 2-methyl-4-chlorophenoxyacetic acid
  • Synthetic method of 2-methyl-4-chlorophenoxyacetic acid
  • Synthetic method of 2-methyl-4-chlorophenoxyacetic acid

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Embodiment 1

[0022] A kind of synthetic method of 2-methyl-4-chlorophenoxyacetic acid, comprises the following steps:

[0023] (1) Preparation of sodium methoxide solution: first add methanol to the reaction flask, then add sliced ​​sodium metal under stirring, react at room temperature for 30 minutes, then heat up to reflux state and keep warm for 30 minutes to obtain sodium methoxide solution;

[0024] (2) Preparation of sodium chloroacetate solution: under stirring, chloroacetic acid is first dissolved in water, after chloroacetic acid is completely dissolved, sodium hydroxide solution is added dropwise at low temperature, when pH=8 is the reaction end point, retest pH=10 minutes later At 8 o'clock, it shows that sodium chloroacetate has been prepared;

[0025] (3) Preparation of o-methylphenoxyacetic acid: add o-methylphenol and sodium methoxide solution to the reaction flask, heat up to reflux under stirring, keep warm for a period of time to remove methanol, remove until the material...

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Abstract

The invention discloses a synthetic method of 2-methyl-4-chlorophenoxyacetic acid and relates to the technical field of organic synthesis. According to the method, o-methylphenol used as a raw material reacts with sodium chloroacetate under the action of sodium methylate; then, a reaction product is neutralized with hydrochloric acid to obtain an intermediate 2-methylphenoxyacetic acid; and finally, the intermediate is subjected to chlorination with sulphone chloride to obtain a target product 2-methyl-4-chlorophenoxyacetic acid. According to the invention, sodium methylate replaces sodium hydroxide to undergo neutralization. The neutralization reaction is relatively thorough, and there are few by-products, thus being beneficial to raise content and yield of the product. In addition, sulphone chloride is used for chlorination. The reaction is a water-free reaction, and generation of lots of phenolic wastewater is minimized. Thus, the reaction meets requirements of modern green pesticides. In addition, reaction temperature is relatively low, thus reducing energy consumption. In comparison with original technologies, the reaction technology has obvious advantages of high yield, less ''three wastes (waste gas, wastewater and industrial residue)'' and low energy consumption.

Description

Technical field: [0001] The invention relates to the technical field of organic synthesis, in particular to a synthesis method of 2-methyl-4-chlorophenoxyacetic acid. Background technique: [0002] There are many types of herbicides currently available on the market, and phenoxyacetic acid herbicides account for an important one. Due to the different substituents and substituent positions on the benzene ring, and the different numbers of carbon atoms of the carboxylic acid, different phenoxycarboxylic acid herbicides are formed. 2-Methyl-4-chlorophenoxyacetic acid is a hormone-type systemic phenoxycarboxylic acid herbicide developed and promoted by Imperial Chemical Industrirs in 1945. It has strong physiological activity on plants and is easy for roots and leaves. surface absorption and conduction. At low concentration, it can stimulate the growth of crops, prevent flower and fruit drop, form seedless fruit, promote fruit ripening and rooting of cuttings, etc.; at high co...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/367C07C59/70C07C51/41C07C51/02C07C51/363C07C51/42
CPCC07C51/367C07C51/02C07C51/363C07C51/412C07C51/42C07C59/70
Inventor 刘兴武蔡永欢尹仕兵肖剑鸣
Owner ANHUI HUAXING CHEM IND CO LTD
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