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Synthesis method of 4-isopropyl-2,5-sodium dimethylbenzenesulfonate

A technology of sodium dimethylbenzenesulfonate and synthetic method, which is applied in the direction of sulfonic acid preparation, sulfonate preparation, organic chemistry, etc., and can solve problems such as low yield and immature synthesis technology

Inactive Publication Date: 2016-07-20
CHANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Sodium 4-isopropyl-2,5-dimethylbenzenesulfonate can be widely used in pesticides to kill insects and weeds, but the synthesis technology is immature and the yield is relatively low

Method used

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  • Synthesis method of 4-isopropyl-2,5-sodium dimethylbenzenesulfonate

Examples

Experimental program
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Effect test

example 1

[0016] First, take 200mL of benzene and put it in a closed container, fill it with nitrogen and add 1g of catalyst aluminum chloride, and add chloromethane with 60% of the mass of benzene to it, seal it and raise the temperature to 105°C, the pressure is raised to 2MPa, and stir After reacting for 2 hours, let it cool down to room temperature naturally, then feed chlorine gas into it, the mass ratio of the amount of feed to benzene is 1:2, and control the speed of feed to 30Ml / s; Add methylmagnesium chloride with 40% of the mass of the mixture, heat it, control the heating temperature to be 40min, and the reaction time is 50min, after the reaction is completed, let it stand, and naturally cool to room temperature; Place it in a four-neck flask equipped with a stirrer, a spherical condenser, and a thermometer, and slowly add 25 mL of sulfuric acid dropwise to it while stirring, control the temperature at 55°C, and heat it at a constant temperature for 30 minutes, then continue t...

example 2

[0018] First, take 150mL of benzene and place it in a closed container, fill it with nitrogen, add 0.5g of catalyst aluminum chloride, and add chloromethane with 50% of the mass of benzene, seal it and heat it up to 100°C, and the pressure is raised to 1.5MPa , after stirring and reacting for 1h, after allowing it to cool naturally to room temperature, feed chlorine gas to it, the mass ratio of the amount fed to benzene is 1:2, and the speed of the feed is controlled to be 25Ml / s; after the feed is completed, Add the methylmagnesium chloride of 30% of mixture quality to it, it is heated, and the control heating temperature is 30min, and the reaction time is 40min, after the completion of the reaction, let it stand, and naturally cool to room temperature; after naturally cooling to room temperature, Put the mixture in a four-necked flask equipped with a stirrer, a spherical condenser, and a thermometer, and slowly add 10 to 25 mL of sulfuric acid dropwise while stirring, control...

example 3

[0020] First, take 170mL of benzene and place it in a closed container, fill it with nitrogen and add 0.7g of catalyst aluminum chloride, and add chloromethane with 55% of the mass of benzene to it, seal and heat up to 104°C, and the pressure rises to 1.7MPa , after stirring and reacting for 1h, after allowing it to cool naturally to room temperature, feed chlorine gas to it, the mass ratio of the amount fed to benzene is 1:2, and the speed of the feed is controlled to be 27Ml / s; after the feed is completed, Add the methylmagnesium chloride of mixture quality 35% to it, it is heated, and the control heating temperature is 35min, and the reaction time is 45min, after the completion of the reaction, let it stand, and naturally cool to room temperature; after naturally cooling to room temperature, Put the mixture in a four-neck flask equipped with a stirrer, a spherical condenser, and a thermometer, and slowly add 25 mL of sulfuric acid dropwise to it while stirring, control the t...

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Abstract

The invention discloses a synthesis method of 4-isopropyl-2,5-sodium dimethylbenzenesulfonate, belonging to the field of organic chemical synthesis. The synthesis method comprises the following steps: firstly putting benzene in a closed container, introducing nitrogen and adding aluminum chloride and methane chloride; sealing and heating; stirring for reacting; naturally cooling; introducing chlorine and adding methyl magnesium chloride; heating, standing and cooling; mixing the mixture with sulfuric acid; heating at constant temperature; putting in deionized water and adjusting the pH value; filtering; adding sodium carbonate into the filtrate; filtering to obtain 2,5-sodium dimethylbenzenesulfonate; putting the 2,5-sodium dimethylbenzenesulfonate into a reaction kettle, adding copper, introducing hydrogen and adding isopropylbenzyl alcohol; and heating, preserving heat, cooling, filtering and drying to obtain the 4-isopropyl-2,5-sodium dimethylbenzenesulfonate. The synthesis method disclosed by the invention has the beneficial effects of simple synthesis conditions, no secondary pollution, few byproducts and relatively high yield.

Description

technical field [0001] The invention discloses a synthesis method of sodium 4-isopropyl-2,5-dimethylbenzenesulfonate, which belongs to the field of organic chemical synthesis. Background technique [0002] Sodium benzenesulfonate is a widely used organic product. White flaky crystals, easily soluble in water, slightly soluble in alcohol. It is used in the synthesis of new pesticides and insecticides, and is used in dye intermediates, detergent auxiliaries and foundry industries. [0003] Sodium 4-isopropyl-2,5-dimethylbenzenesulfonate can be widely used in pesticides to kill insects and weeds, but the synthesis technology is immature and the yield is relatively low. Contents of the invention [0004] The invention provides a method for synthesizing sodium 4-isopropyl-2,5-dimethylbenzenesulfonate with mild reaction conditions and high yield. [0005] In order to achieve the above object, a kind of synthetic route of 4-isopropyl-2,5-dimethylbenzenesulfonate sodium of the ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C309/31C07C303/32
CPCC07C303/32C07C303/06
Inventor 董燕敏
Owner CHANGZHOU UNIV
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