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Purification method of new 2-nitro-4-methylsulfonylbenzoic acid

A technology of methanesulfonyl benzoic acid and purification method, which is applied in chemical instruments and methods, organic chemistry, preparation of organic compounds, etc., can solve problems such as high cost and complicated operation, and achieve the effects of easy operation and low purification cost.

Inactive Publication Date: 2017-05-24
NUTRICHEM LAB CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] Patent CN1500077 also discloses a purification method of 2-nitro-4-methylsulfonylbenzoic acid, which hydrolyzes unnecessary dinitro-substituted impurities by adjusting pH, adsorbing on activated carbon, and later alkali treatment , but this method is complex to operate in actual industrial production and the cost is high

Method used

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  • Purification method of new 2-nitro-4-methylsulfonylbenzoic acid

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Embodiment 1

[0026] 50 grams of 2-nitro-4-methylsulfonylbenzoic acid crude product was added in 150 milliliters of methanol of 90% content, and the temperature was raised to 67° C., and the material was completely dissolved and filtered under reflux, then slowly cooled, and gradually cooled to 5 ℃, wait until the product is completely precipitated, filter, take the filter cake, and dry to obtain the product.

Embodiment 2

[0028] Add 50 grams of crude 2-nitro-4-methylsulfonylbenzoic acid to 150 milliliters of absolute ethanol, raise the temperature to 78° C., dissolve and filter the material under reflux, add 30 milliliters of n-hexane, and then slowly lower the temperature. Gradually cool to 5°C, wait until the product is completely precipitated, filter, take the filter cake, and dry to obtain the product.

Embodiment 3

[0030] Add 50 grams of 2-nitro-4-methylsulfonylbenzoic acid crude product into 150 ml of dichloromethane, heat up to 65°C, dissolve and filter the material under reflux, then slowly cool down, and gradually cool to 0°C, After the product is completely precipitated, filter, take the filter cake, and dry to obtain the product.

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Abstract

The present invention discloses a purification method of new 2-nitro-4-methylsulfonylbenzoic acid. The specific method comprises the following steps: 1) crude 2-nitro-4-methylsulfonylbenzoic acid products are put into an appropriate amount of solvent, the crude products are heated to be 30-150 DEG C in a stirring condition; 2) precipitation temperature is reduced until the products are completely precipitated; and 3) the precipitated products are filtered and filtering cakes are taken to obtain the products. The purity of the 2-nitro-4-methylsulfonylbenzoic acid purified by the technical scheme is more than or equal to 98.5%, and the contents of the key impurities are greatly reduced. At the same time, the technical scheme is very easy to operate, relatively low in purification costs and conductive to be used for industrial productions.

Description

technical field [0001] The invention relates to the field of pesticide production, in particular to the synthesis and purification of an intermediate 2-nitro-4-methylsulfonylbenzoic acid of the pesticide mesotrione. Background technique [0002] 2-Nitro-4-methylsulfonylbenzoic acid is an important intermediate in the synthesis of the pesticide mesotrione, a broad-spectrum preemergence and postemergence inhibitor of hydroxyphenylpyruvate dioxygenase Selective herbicide, effective against broadleaf grasses and some grasses. The molecular structural formula of 2-nitro-4-methylsulfonylbenzoic acid is: [0003] [0004] At present, the main synthetic routes of 2-nitro-4-methylsulfonylbenzoic acid include the following: 1) take toluene as raw material, and then synthesize the product through the steps of nitration, oxidation, sulfuration and then re-oxidation; 2) use p-mercapto Toluene is used as a raw material, and mercapto groups are first methylated, and synthesized throug...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C315/06C07C317/44
CPCC07C315/06C07C317/44
Inventor 王磊倪肖元谭徐林尚丽霞
Owner NUTRICHEM LAB CO LTD
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