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A kind of synthetic method of 3,6-dichloro-2-methoxybenzoic acid

The technology of a methoxybenzoic acid and a synthesis method is applied in the synthesis field of 3,6-dichloro-2-methoxybenzoic acid, and can solve the problems of high difficulty in industrialization, large discharge of three wastes, long reaction steps and the like, Achieve the effects of good product quality, reduced waste water, and short steps

Active Publication Date: 2016-04-27
浙江拜克生物科技有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0009] Each of the above-mentioned process routes has its own shortcomings. Some reactions have high requirements, harsh conditions, and industrialization is difficult; some reaction steps are long, the post-treatment is complicated, the yield is low, and the discharge of three wastes is large

Method used

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  • A kind of synthetic method of 3,6-dichloro-2-methoxybenzoic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] 1) In a 500ml four-neck flask, dissolve 36g (98.5%) of 2,5-dichloroanisole in 100ml of dichloromethane, and add 0.2g of TiCl 4 , lower the temperature to 5°C, slowly add 100ml of methylene chloride solution containing 27.84g (99%) of dichloromethyl methyl ether dropwise under stirring conditions, add 200ml of water after the addition is completed, and adjust the pH to 3.0 with dilute sulfuric acid, at 25°C Stir for 4h. After standing still, the oil layer was separated to obtain 40.2 g of 2-methoxy-3,6-dichlorobenzaldehyde with a yield of 95%.

[0026] 2) Add 150ml of toluene solution of 21g (98%) 2-methoxy-3,6-dichlorobenzaldehyde into a 500ml four-necked flask, slowly add 24.9g of 30% NaClO solution under stirring condition, and control the temperature at 25°C , Stir the reaction for 5h. Toluene was distilled off under reduced pressure, dilute sulfuric acid was added to the aqueous solution to adjust the pH to 1.0, the temperature was lowered, and after filtration an...

Embodiment 2

[0028] 1) In a 500ml four-neck flask, dissolve 37g (97.0%) of 2,5-dichloroanisole in 100ml of dichloroethane, and add 0.4g of TiCl 4 , lower the temperature to 10°C, maintain the temperature, and slowly add 100ml of dichloroethane solution containing 21.0g (99%) of dichloromethyl methyl ether dropwise under stirring conditions, add 300ml of water after the addition is completed, and adjust the pH to 1.5 with sulfuric acid , Stir at 20°C for 3h. After standing still, the oil layer was separated to obtain 39.2 g of 2-methoxy-3,6-dichlorobenzaldehyde, with a yield of 93.7%.

[0029] 2) Add 21g (98%) 2-methoxy-3,6-dichlorobenzaldehyde in 150ml of dichloroethane solution into a 500ml four-necked flask, slowly add 60g of 20% NaBrO solution under stirring condition, and control the temperature 20 ° C, stirring the reaction for 3h. Dichloroethane was distilled off under reduced pressure, and an appropriate amount of dilute sulfuric acid was added to the remaining aqueous solution to...

Embodiment 3

[0031] 1) In a 500ml four-neck flask, dissolve 37g (97.0%) of 2,5-dichloroanisole in 100ml of toluene, and add 0.3g of TiCl 4 , cool the cold brine to 0°C, slowly add 100ml of toluene solution dissolved with 26g of dichloromethyl methyl ether dropwise under stirring conditions, add 100ml of water after the dropwise addition, adjust the pH to 2.0 with sulfuric acid, and stir at 15°C for 6h. After standing still, the oil layer was separated to obtain 39.8 g of 2-methoxy-3,6-dichlorobenzaldehyde, with a yield of 95.14%.

[0032] 2) Add 150ml of dichloroethane solution of 21g (98%) 2-methoxy-3,6-dichlorobenzaldehyde into a 500ml four-neck flask, slowly add 15g of 30% hydrogen peroxide solution under stirring condition, and control the temperature 15°C, stirred and reacted for 8h. The solvent was distilled off under reduced pressure, and an appropriate amount of dilute sulfuric acid was added to the remaining aqueous solution to adjust the pH to 2.0. After filtration and drying, 2...

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Abstract

The present invention relates to a method for the synthesis and preparation of the herbicide 3,6-dichloro-2-methoxybenzoic acid (i.e. dicamba), which is realized by the following steps: 1) formylation of 2,5-dichloroanisole , to obtain 2-methoxy-3,6-dichloroanisole; 2) Oxidation of 2-methoxy-3,6-dichloroanisole, the reaction product was acidified, filtered and dried to obtain the product. The process has high product yield, does not use high-pressure carboxylation reaction, solves the problem of large discharge of three wastes in the existing production process, has good environmental protection benefits, is easy to industrialize, and has good application value.

Description

technical field [0001] The present invention relates to a method for the synthesis and preparation of a herbicide - 3,6-dichloro-2-methoxybenzoic acid (i.e. dicamba), in particular to a green and environment-friendly 3,6-dichloro-2-methoxybenzoic acid The synthetic method of oxybenzoic acid. technical background [0002] 3,6-dichloro-2-methoxybenzoic acid, namely dicamba (Dicamba), also known as Baquat. Belonging to benzoic acid herbicides, it has the characteristics of broad spectrum, high efficiency and low toxicity; it has strong weeding selectivity, less dosage and low cost. It is mainly used to control annual or perennial broad-leaved weeds in the fields of wheat and other gramineous plants, such as pig scorpion, buckwheat vine, quinoa, beef chickweed, wormwood, cocklebur, spinach, vetch, shepherd's purse, etc. kind. Dicamba has a systemic conduction effect. It is used for post-emergence spraying. The medicine is quickly absorbed by the leaves, stems and roots of the...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C51/16C07C51/285C07C65/21
CPCC07C41/30C07C45/43C07C51/16C07C51/285C07C65/21C07C47/575C07C43/225
Inventor 葛庆余余中宝徐红彪朱卫军章明莲罗晓芳张华弟
Owner 浙江拜克生物科技有限公司
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