Method for synthesizing o-methyl formate benzene sulfonamide

A technology of methyl o-formate benzenesulfonamide and methyl ester, applied in the direction of sulfonamide preparation, sustainable manufacturing/processing, chemical industry, etc., can solve the complex production process of o-methyl benzenesulfonamide, environmental pollution, cost Advanced problems, to achieve the effect of saving raw materials, saving energy, and low cost

Inactive Publication Date: 2012-07-25
王继龙
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Problems solved by technology

[0003] For above-mentioned situation, in order to overcome the defective of prior art, the object of the present invention provides a kind of method of synthesizing methyl o-formate benzene sulfonamide, can effectively solve the complex production process of o-methyl o-formate benzene sulfonamide, high cost, low efficiency and the problem of polluting the environment

Method used

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  • Method for synthesizing o-methyl formate benzene sulfonamide
  • Method for synthesizing o-methyl formate benzene sulfonamide
  • Method for synthesizing o-methyl formate benzene sulfonamide

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Embodiment Construction

[0019] The specific implementation manners of the present invention will be described in detail below in conjunction with the accompanying drawings.

[0020] In concrete implementation, the present invention is realized by the following steps:

[0021] 1. Preparation of the methyl ester mixture:

[0022] Put 480 kg of water into the dissolving pot, heat to 25-30°C, add 150kg of sodium nitrite under stirring, dissolve, then add 320kg of methyl anthranilate, stir at 30°C for 15 minutes to obtain a mixture of methyl esters;

[0023] 2. Diazo reaction:

[0024] (1) Prepare mixed acid: put 320kg of water into the diazo pot, add 167kg of sulfuric acid (H 2 SO 4 ), adding 605kg of hydrochloric acid (HCl) at a temperature ≤ 35°C to obtain a mixed acid with an acidity of 39.5-47 g / 100ml (due to the temperature, the quality of sulfuric acid and hydrochloric acid will cause the concentration of the mixed acid to be unstable, if the mixed acid If the concentration is less than 39.5-4...

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Abstract

The invention relates to a method for synthesizing o-methyl formate benzene sulfonamide which is capable of effectively solving the problems that a conventional o-methyl formate benzene sulfonamide synthesizing method is complex in process, high in cost, low in efficiency and pollutes environment and comprises the steps of: heating water, adding sodium nitrite, dissolving, and adding methyl o-aminobenzoate to obtain a methyl ester mixture; putting the water in a diazo pot, adding sulfuric acid and hydrochloric acid to obtained mixed acid; reducing the temperature of the mixed acid, adding the methyl ester mixture, reacting to obtain a diazonium salt solution, adding copper sulfate, introducing sulfur dioxide, determining by utilizing an H acid reagent solution and fading by utilizing the H acid; adding toluene, introducing liquid chlorine, determining to be darkgreen by utilizing a benzidine reagent solution, standing and layering to obtain an o-methyl formate benzene sulfonamide solution at the upper layer; and adding anhydrous toluene and carbinol, introducing liquid ammonia, adjusting pH (potential Of Hydrogen) value to be neutral by using acetic acid, removing the acetic acid, washing till being colourless by using the toluene, removing the toluene, beating by using the water, washing to be neutral, removing the water and drying. The method disclosed by the invention has the advantages of easiness in operation, high efficiency, low cost and good quality, and saves energy and raw material, and is environment-friendly.

Description

technical field [0001] The invention relates to chemical industry, in particular to a method for synthesizing methyl o-formate benzenesulfonamide (also known as methanesulfonamide). Background technique [0002] Methyl o-formate benzenesulfonamide (methylsulfonamide) is an important pesticide and pharmaceutical intermediate, mainly used in the synthesis of sulfonylurea herbicides. Among them, there is a class of products such as sulfonylurea herbicides such as chlorimsulfuron-methyl, sulfasulfuron-methyl, flurimsulfuron-methyl, propoxysulfuron-methyl, metsulfuron-methyl, tribenuron-methyl, metsulfuron-methyl and other varieties of sulfonylurea herbicides and methyl-o-formate It is one of the main raw materials for the synthesis of the above herbicides. Its traditional synthesis method is obtained by esterification of o-benzoylsulfonimide (saccharin) and methanol. The method is to obtain methyl o-formate benzenesulfonyl chloride, aminate it with ammonia water to form an amin...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C311/16C07C303/38
CPCY02P20/10
Inventor 王继龙
Owner 王继龙
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