Methyl p-tolyl sulfone and preparation method

A technology of methylsulfonyltoluene and p-toluenesulfonyl chloride is applied in the fields of pesticides, raw material intermediates and preparation, medicine, veterinary drugs, and dyestuffs. The effect of pollution risk, reduction of raw material cost, and simple production process

Inactive Publication Date: 2017-02-22
沈根荣
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

To prepare p-thymphenyltoluene, because p-thymphenyltoluene is a highly toxic drug, which is extremely harmful to the body and the environment, so it is not suitable for manual operation; with the strict control of highly toxic drugs, the price is also gradually rising. Therefore, the original traditional three process preparation methods have been gradually replaced by new production processes; such as the Chinese invention patent application with the application number 2008101626197 and the name "production process of p-thiamphenyl toluene", the p-thiamphenyl toluene produced by it The toluene product yield is 65%-70%, and the content is 99%. Quality: light brown powdery crystal; its disadvantages are: low content, low yield, poor quality, high impurity content, large consumption of raw and auxiliary materials, energy consumption ( Electricity, steam) high, long production cycle

Method used

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  • Methyl p-tolyl sulfone and preparation method
  • Methyl p-tolyl sulfone and preparation method
  • Methyl p-tolyl sulfone and preparation method

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preparation example Construction

[0036] figure 1 Shown, a kind of p-thiamphenicol toluene preparation method of the present invention, described preparation method comprises the steps:

[0037] a) Add water to the salt forming kettle in proportion, start stirring and heat up to 32°C-35°C, add sodium carbonate, anhydrous sodium sulfite, and p-toluenesulfonyl chloride in proportion, and let the materials react naturally after closing the manhole, and the time is 40 -60 minutes;

[0038] b) After the salt-forming reaction is finished, feed steam to raise the temperature to 78°C-82°C, turn off the steam and keep it warm for 50-70 minutes to prepare a sodium p-toluenesulfinate solution;

[0039] c) After the heat preservation is over, open the manhole, add 150-250 mesh activated carbon in proportion under stirring, heat filtration for 10-30 minutes, reflux, and after the solution is completely clarified, directly replace it into the methylation reaction kettle;

[0040] d) After the filtration is finished, feed ...

Embodiment 2

[0050] In the step a), add 2000kg of water to the salt-forming kettle in proportion, start stirring and heat up to 32°C, add 290kg of sodium carbonate, 330kg of anhydrous sodium sulfite, and 450kg of p-toluenesulfonyl chloride at one time, and let the The material reacts naturally, and the time is 40 minutes;

[0051] In step b), after the salt-forming reaction is completed, the temperature in the kettle rises to between 65°C and 75°C, and steam is introduced to raise the temperature to 78°C, and the steam is turned off to keep the temperature for 50 minutes to prepare a sodium p-toluenesulfinate solution;

[0052] In step c), after the heat preservation is finished, open the manhole, add 150 mesh activated carbon in proportion under stirring, and stir for 10 minutes to carry out hot filtration;

[0053] In step d), after the filtration is completed, feed steam to raise the temperature, close the steam at 82°C, open the methyl chloride pipeline valve to carry out the methylati...

Embodiment 3

[0056] Embodiment 3: In the described step a), add 2200kg of water in the salt forming kettle in proportion, start stirring and heat up to 35°C, throw in 330kg of sodium carbonate, 390kg of anhydrous sodium sulfite, and 550kg of p-toluenesulfonyl chloride at one time, and close the After the manhole, let the material react naturally for 60 minutes;

[0057] In step b), after the salt-forming reaction is completed, the temperature in the kettle rises to between 65°C and 75°C, the temperature is raised to 82°C by feeding steam, and the steam is turned off for 70 minutes to prepare a sodium p-toluenesulfinate solution;

[0058] In step c), after the heat preservation is finished, open the manhole, add 250 mesh activated carbon in proportion under stirring, and stir for 30 minutes to carry out hot filtration;

[0059] In step d), after the filtration is completed, feed steam to raise the temperature, close the steam at 85°C, open the methyl chloride pipeline valve to carry out the...

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Abstract

The invention discloses methyl p-tolyl sulfone and a preparation method. Methyl p-tolyl sulfone is prepared from components of raw and auxiliary materials in parts by weight as follows: 200 parts of water, 29 parts of sodium carbonate, 33 parts of anhydrous sodium sulfite, 45 parts of paratoluensulfonyl chloride, 1 part of activated carbon, 3 parts of sodium hydroxide and 16 parts of chloromethane. The preparation method comprises steps as follows: a) water is added to a salt formation kettle in proportion, stirring is started, sodium carbonate, anhydrous sodium sulfite and paratoluensulfonyl chloride are added once in proportion after heating, and the materials naturally react after a manhole is tightly closed; b) steam is introduced, heating and thermal insulation are performed, and a paratoluensulfonyl chloride solution is prepared; c) activated carbon is added in proportion during stirring, hot filtration is performed during stirring, and the mixture is subjected to direct replacement and then enters a methylation reaction kettle; d) steam is introduced, heating is performed, a chloromethane pipeline valve is opened for a methylation reaction; a methylation reduction reaction is performed again after thermal insulation; e) sodium hydroxide is sucked once for a neutralization reaction; f) the mixture is transferred into a centrifugal machine to be spin-dried and then transferred into an oven to be dried.

Description

technical field [0001] The invention relates to p-thymphenyltoluene and a preparation method thereof, and belongs to the technical fields of medicine, veterinary medicine, pesticide, dyestuff, raw material intermediate and preparation. Background technique [0002] P-thymphenyltoluene is an important intermediate of new medicine, veterinary medicine, pesticide and dyestuff promoted by the state. Appearance white crystal, melting point 86°C-88°C, insoluble in water, soluble in common organic solvents. It is designated as the intermediate of the new broad-spectrum antibiotic thiamphenicol, and also the intermediate of fluprofen, mesotrione, and sulcotrione. In foreign countries, it is widely allowed to be used in immunosuppressive state antibiotics, as well as food and feed additives, etc., and the market demand is increasing year by year. [0003] At present, the domestic production of p-thiamphenicol toluene as raw materials for medicine, veterinary drugs and pesticides is...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C315/04C07C315/06C07C317/14
CPCC07C315/04C07C315/06C07C317/14
Inventor 沈根荣
Owner 沈根荣
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