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A synthesis method and technology of dicamba are applied in the field of synthesis of dicamba and the preparation of herbicide dicamba, which can solve the problems of high requirement of reaction conditions, long reaction time and high energy consumption, and achieve the reaction process of green environmental protection, good quality, high yield effect
Inactive Publication Date: 2012-12-26
SHANDONG WEIFANG RAINBOW CHEM
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Problems solved by technology
At present, this method is mostly used in industry for production, but its disadvantages are long reaction time and high energy consumption.
This method requires high reaction conditions and a long time
Method used
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Embodiment 1
[0026] Add 32.7g of 99% 2,5-dichlorophenol to 90g of 92.5% sulfuric acid, heat to 120°C and stir for 3h. After the reaction was completed, it was lowered to room temperature, and the precipitated white crystals were filtered with suction, washed with a small amount of methanol, and dried to obtain 47.7g of 4-hydroxy-2,5-dichlorobenzenesulfonic acid, with a yield of 98.5%.
Embodiment 2
[0028]Add 32.7g of 99% 2,5-dichlorophenol into 80g of 98% sulfuric acid, heat to 150°C and stir for 2h. After the reaction was completed, it was lowered to room temperature, and the precipitated white crystals were filtered with suction, washed with a small amount of methanol, and dried to obtain 47.8 g of 4-hydroxy-2,5-dichlorobenzenesulfonic acid, with a yield of 98.8%.
Embodiment 3
[0030] 32.7g of 99% 2,5-dichlorophenol was added to 41.6g of 94% sulfuric acid, heated to 200°C and stirred for 5 hours. After the reaction was completed, it was lowered to room temperature, and the precipitated white crystals were filtered with suction, washed with a small amount of methanol, and dried to obtain 45.5 g of 4-hydroxy-2,5-dichlorobenzenesulfonic acid, with a yield of 94.0%.
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Abstract
The invention discloses a synthesis method of dicamba, which comprises the following steps of: using 2, 5-dichlorophenol as raw materials, conducting sulfonation and bromination reaction to obtain 4-hydroxy-2, 5-dichloro-3-bromobenzenesulfonic acid, treating the 4-hydroxy-2, 5-dichloro-3-bromobenzenesulfonic acid by using alkyl metal complexes of magnesium or lithium, conducting electrophilic addition reaction with CO2 to obtain 5-sulfo-3, 6-diclorsalicylic acid, removing the sulfo of the 5-sulfo-3, 6-diclorsalicylic acid and conducting O-methylation reaction with methyl chloride to obtain the dicamba. The synthesis method of dicamba has the advantages that since the 2, 5-dichlorophenol is used as the raw materials, the raw materials for reaction are easy to obtain, the reaction process is environmental-friendly, the quality of the obtained product is high, the yield is high and the application value is greater.
Description
technical field [0001] The invention relates to a method for preparing a herbicide dicamba, in particular to a method for synthesizing a green and environment-friendly dicamba, which belongs to the technical field of herbicides. Background technique [0002] Dicamba (Dicamba), also known as Baicao, chemically named 3,6-dichloro-2-methoxybenzoic acid, is a low-toxic, high-efficiency, broad-spectrum benzoic acid herbicide with strong selectivity and It is characterized by less quantity and low cost, and is mainly used for the control of annual or perennial broad-leaved weeds in the field of wheat and other gramineous crops, such as pigtail, vetch, buckwheat vine, quinoa, chickweed, cow chickweed, sow There are more than 200 kinds of nymphs, cockleburs, field bindweed, thorns, thorns, scallops, leeks, snakehead sausages, shepherd's purse, and Polygonum. The original drug content is more than 98%, and the main dosage forms are 48% water, 40% wettable powder and compound dosage ...
Claims
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