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Industrialized production method for methyl p-tolyl sulfone

A technology of thiamphenyl toluene and p-thymphenyl toluene, which is applied in the field of industrial production of p-thymphenyl toluene, and can solve the problems of large equipment investment, heavy labor stress, and high labor intensity.

Active Publication Date: 2012-02-29
浙江嘉化新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The use of batch-type reactors will cause serious environmental pollution, high labor intensity, and large equipment investment.
[0003] The Chinese patent title of the application number 200810162619.7 is "the production process of p-thiamphenicol", and the Chinese patent title of the application number 200910018412.7 is "the preparation method of p-thiamphenyl toluene". Both methods use batch reactors , the labor stress is great, and the pollution to the environment is also relatively large
[0004] Application number is 200910018223.X Chinese patent title is " a kind of preparation method of thiamphenicol toluene ", and its shortcoming is that needs to add activated carbon to carry out circulating reflux filtration in reaction process, and technology is more complicated, is unfavorable for the process of industrialization, and Refining with this method will reduce the yield of the product

Method used

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  • Industrialized production method for methyl p-tolyl sulfone
  • Industrialized production method for methyl p-tolyl sulfone

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Anhydrous sodium sulfite, sodium bicarbonate, p-toluenesulfonyl chloride and water are continuously put into the primary reduction reaction kettle according to the mass ratio of 0.72:1:1:3. The feed rate of p-toluenesulfonyl chloride is 490kg / h, the feed rate of anhydrous sodium sulfite is 352.8kg / h, the feed rate of sodium bicarbonate is 490kg / h, and the feed rate of water is 1470kg / h. The stirring is started, the temperature of the primary and secondary reduction reactors is maintained at 50-60°C, and the temperature of the third-stage reduction reactor is maintained at 70-80°C. The material enters the secondary reactor from the overflow port of the primary reactor, and then enters the third-stage heating reactor. Then enter the methylation multi-tank series system.

[0032] The material entering the stainless steel methylation kettle automatically flows from the liquid in the previous kettle to the next kettle through overflow in the methylation kettle, and graduall...

Embodiment 2

[0036]Anhydrous sodium sulfite, sodium bicarbonate, p-toluenesulfonyl chloride and water are continuously put into the primary reduction reaction kettle according to the mass ratio of 0.72:1:1:3. The feed rate of p-toluenesulfonyl chloride is 490kg / h, the feed rate of anhydrous sodium sulfite is 352.8kg / h, the feed rate of sodium bicarbonate is 490kg / h, and the feed rate of water is 1470kg / h. The stirring is started, the temperature of the primary and secondary reduction reactors is maintained at 50-60°C, and the temperature of the third-stage reduction reactor is maintained at 70-80°C. The material enters the secondary reactor from the overflow port of the primary reactor, and then enters the third-stage heating reactor. Then enter the methylation multi-tank series system.

[0037] The material entering the stainless steel methylation kettle automatically flows from the liquid in the previous kettle to the next kettle through overflow in the methylation kettle, and gradually...

Embodiment 3

[0041] Anhydrous sodium sulfite, sodium bicarbonate, p-toluenesulfonyl chloride and water are continuously put into the primary reduction reaction kettle according to the mass ratio of 0.72:1:1:3. The feed rate of p-toluenesulfonyl chloride is 490kg / h, the feed rate of anhydrous sodium sulfite is 3528kg / h, the feed rate of sodium bicarbonate is 490kg / h, and the feed rate of water is 1470kg / h. The stirring is started, the temperature of the primary and secondary reduction reactors is maintained at 50-60°C, and the temperature of the third-stage reduction reactor is maintained at 70-80°C. The material enters the secondary reactor from the overflow port of the primary reactor, and then enters the third-stage heating reactor. Then enter the methylation multi-tank series system.

[0042] The material entering the methylation tank automatically flows from the liquid in the previous tank to the next tank through overflow in the methylation tank, and gradually participates in the rea...

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Abstract

An industrialized production method for methyl p-tolyl sulfone comprises the following steps of: carrying out reduction reaction to p-toluenesulfonyl chloride and anhydrous sodium sulphite as well as sodium bicarbonate in a tertiary serial reduction reaction kettle, generating p-methyl sodium sulphinate; methylating the p-methyl sodium sulphinate into the methyl p-tolyl sulfone by chloromethane in a tertiary serial methylation kettle; separating an organic layer by a tertiary liquid separating tower; and preparing a methyl p-tolyl sulfone product through washing, crystallizing and dewatering. In the invention, dimethyl sulfate as a highly toxic chemical is not adopted to avoid the harm to human bodies and environment; and as a multi-kettle serial technology is adopted for reduction salification reaction and methylation reaction, p-toluenesulfonyl chloride salification and methyl p-tolyl sulfone synthesis can be completely reacted to realize continuous production.

Description

technical field [0001] The invention relates to an industrialized production process of a pharmaceutical intermediate sulfone, and an industrialized production method of p-thiamphenicol toluene. Background technique [0002] p-thiamphenicol toluene is the main raw material for the production of p-thiamphenicol beseramide, and p-thiamphenicyl beseramide is the main raw material for the synthesis of national second-class new drugs, forprofen and thiamphenicol. huge demand. The existing mature production process of p-thiamphenicol toluene adopts batch reaction kettle, takes p-toluenesulfonyl chloride as raw material, reduces sodium sulfite to sodium p-toluenesulfinate, and then uses dimethyl sulfate for methylation reaction. Made of p-methylsulfonyl toluene. Dimethyl sulfate is highly toxic and has great harm to human body and environment. The use of batch-type reactors will cause serious environmental pollution, high labor intensity, and large equipment investment. [0003...

Claims

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Application Information

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IPC IPC(8): C07C317/14C07C315/00
Inventor 王宏亮赵丽丰沈高庆胡文俊蒋勤明冯明红
Owner 浙江嘉化新材料有限公司
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