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Preparation method of benzoic acid herbicide dicamba

A technology of herbicides and dicamba, applied in the preparation of carboxylate salts, preparation of organic compounds, chemical instruments and methods, etc.

Inactive Publication Date: 2012-06-27
JIANGSU CHANGQING AGROCHEMICAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] 4. In Japanese Patent JP4805574, 2,5-dichlorophenol was used as raw material to obtain 2 through etherification, Claisen rearrangement, etherification and oxidation -Methoxy-3,6-dichlorobenzoic acid, its preparation method is ingenious, but its yield is low, and a large amount of three wastes are produced, so the cost is relatively high, and it has not been adopted in industrial production

Method used

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Examples

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Embodiment Construction

[0026] One, the synthetic method of 2,5-dichlorophenyl acetate:

[0027] 1. Add 83.32g, 0.5mol 2,5-dichlorophenol (purity 99%) 500ml of toluene solution to a 1000ml four-necked bottle equipped with mechanical stirring, thermometer, condenser, dropping funnel, and water separator, 30.4 g, 0.5mol potassium hydroxide (purity 92%) began to heat up to reflux for about 5 to 6 hours, separated 9 grams of water, and a large amount of white flocculent solids were precipitated in the bottle as potassium 2,5-dichlorophenate, and then cooled to After cooling down at room temperature with a water bath, add 40.9 g.0.51 mol of acetyl chloride (purity 98%) dropwise for about 2 hours. The white flocculent solid disappears, and a white powdery solid precipitates out. Sampling and gas spectrometry analysis. When the 2,5-dichlorophenol was finished, it was filtered, and the mother liquor was distilled to give a dark yellow solid of 103 grams of 2,5-dichlorophenyl acetate, with a content o...

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PUM

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Abstract

A preparation method of a benzoic acid herbicide dicamba relates to the technical filed of pesticide production. The invention employs 2,5-dichlorophenols as a raw material and carries out esterification, Fries rearrangement, etherification and oxidation to obtain 3,6-dichloro-2-methoxybenzoic acid. The synthetic method has simple technology, easily available raw material, low cost, generates little "three wastes (waste gas, waste water and industrial residue)" and is more environment-friendly and more suitable for industrialized production.

Description

technical field [0001] The invention relates to the technical field of pesticide production. Background technique [0002] Dicamba, scientific name 3,6-dichloro-2-methoxybenzoic acid, belongs to the series of benzoic acid herbicides and is a relatively friendly herbicide to the environment. Its production method mostly uses the potassium salt of 2,5-dichlorophenol and carbon dioxide under high pressure conditions to carry out carboxylation, re-esterification, and hydrolysis to obtain dicamba. [0003] In recent years, there are few reports on the synthesis methods of 3,6-dichloro-2-methoxybenzoic acid (dicamba), but there are many reports on its preparation methods in the 1950s to 1970s. The synthesis methods are generally summarized as follows . [0004] 1. In the patent document Ussr345129, 1973; Po1:78848, 1975; us4161611, 2-amino-3,6-dichlorobenzoic acid is used as raw material to synthesize 3,6 after diazotization and etherification with methyl chloride - Dichloro-2-...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C65/21C07C51/255
Inventor 于国权吉志扬张振明王建荣丁华平
Owner JIANGSU CHANGQING AGROCHEMICAL CO LTD
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