Synthesis method of 1-methyl-4-methyl sulfonyl benzene

A technology of methylsulfonylbenzene and a synthesis method, which is applied in chemical instruments and methods, chemical methods for reacting liquids and gaseous media, and preparation of organic compounds, etc. to prevent material blockage and enhance the gas-liquid contact reaction

Pending Publication Date: 2018-03-23
浙江嘉化新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
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Problems solved by technology

This process technology uses methyl chloride gas to ventilate from the third-stage reactor, then to the second-stage reactor, and then to the first-stage reactor. The pressure in each reactor is unbalanced, which is not conducive to the outflow of liquid, and it is not easy to carry out the reaction. Three-stage liquid separation tower, material clogging is serious

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  • Synthesis method of 1-methyl-4-methyl sulfonyl benzene

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preparation example Construction

[0016] Such as figure 1 As shown, the reaction of methyl chloride and sodium 4-toluenesulfinate generates 1-methyl-4-methylsulfonylbenzene, and the steps of the synthesis method of 1-methyl-4-methylsulfonylbenzene of the present invention are:

[0017] a. Synthesis of 1-methyl-4-methylsulfonylbenzene: Sodium 4-toluenesulfinate enters into 1 through delivery pump 1 # In methylation kettle 2, methyl chloride gas enters into 1 by bubbling # Inside the methylation kettle 2, 1 # In the methylation kettle, the mixed reaction is carried out by self-priming stirring 6, and the reacted material is from 1 # The overflow port on the upper side of the methylation kettle 2 flows into and out of the 2 # In methylation kettle 3, methyl chloride gas enters into 2 by bubbling # In the methylation kettle 3, unreacted 4-sodium toluene sulfinate and methyl chloride are mixed and reacted by self-priming stirring 7, and the reacted material is from 2 # The overflow port on the upper side of th...

Embodiment 1

[0033] Put 4-sodium toluene sulfinate into 1 via delivery pump # In the methylation still, pass into methyl chloride gas, stir reaction, the mixed material after reaction is from 1 # Methylation kettle overflowed to 2 # Methylation still, pass into chloromethane gas to 2 # Methylation tank, stirring reaction, the mixed material after reaction from 2 # Methylation tank overflow into 3 # Methylation kettle, methyl chloride gas into 3 # Methylation tank, stirring reaction, after the reaction, the mixed material is from 3 # Methylation tank overflow into 4 # Methylation kettle, feed into the methyl chloride gas, stir the reaction, the reaction temperature of the four reactors is 92°C, the reaction pressure is 0.45MPa, the liquid level is ≤90%, from 4 # Samples were taken from the bottom of the methylation kettle, and the content of sodium 4-toluenesulfinate in the reaction liquid was analyzed by liquid chromatography. The content was 0.05%. After the reaction was completed, ...

Embodiment 2

[0037] Put 4-sodium toluene sulfinate into 1 via delivery pump # In the methylation still, pass into methyl chloride gas, stir reaction, the mixed material after reaction is from 1 # Methylation kettle overflowed to 2 # Methylation still, pass into chloromethane gas to 2 # Methylation tank, stirring reaction, the mixed material after reaction from 2 # Methylation tank overflow into 3 # Methylation kettle, methyl chloride gas into 3 # Methylation tank, stirring reaction, after the reaction, the mixed material is from 3 # Methylation tank overflow into 4 # Methylation tank, feed into methyl chloride gas, stir reaction, the reaction temperature of the four reactors is 90°C, the reaction pressure is 0.5MPa, the liquid level is ≤90%, from 4 # Samples were taken from the bottom of the methylation kettle, and the content of sodium 4-toluenesulfinate in the reaction liquid was analyzed by liquid chromatography. The content was 0.05%. After the reaction was completed, a 1-methyl-...

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Abstract

The invention discloses a method for synthesizing 1-methyl-4-methylsulfonylbenzene, which involves stirring sodium 4-toluenesulfinate and methyl chloride through a four-stage methylation reaction to obtain 1-methyl-4 ‑Methylsulfonylbenzene mixed solution, after the mixed solution enters the separatory tower to stand and separate, then obtains 1‑methyl‑4‑methylsulfonylbenzene product through washing, crystallization and dehydration. The present invention adopts self-priming stirring, stirring Negative pressure is generated when the device itself rotates in the liquid. Under negative pressure, methyl chloride gas is sucked in to enhance the gas-liquid contact reaction, so that the reaction is complete, and the pressure on the surface of the four methylation kettles is guaranteed to be the same to ensure that the liquid in the kettle is fully The overflow adopts a single-stage liquid separation tower, which prevents material clogging and realizes continuous production.

Description

technical field [0001] The invention belongs to the technical field of organic chemistry, and in particular relates to a synthesis method of 1-methyl-4-methylsulfonylbenzene. Background technique [0002] 1-methyl-4-methylsulfonylbenzene is widely used in the synthesis of pharmaceutical antibiotic thiamphenicol, pesticide herbicide mesotrione and organic synthesis intermediates, and has considerable application value. At present, there is a mature method for synthesizing 1-methyl-4-methylsulfonylbenzene. Sodium 4-toluenesulfinate is obtained through the methylation reaction of dimethyl sulfate. Dimethyl sulfate is a highly toxic drug that is harmful to the human body. It is very harmful to the environment, and the use of batch reactors will cause great environmental pollution and high labor intensity. [0003] The patent application number is 201110360094.X, and the Chinese patent name is "method for preparing 4-thiamphenicol toluene". The ammonium salt ionic liquid is pre...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C315/00C07C317/14B01J19/18B01J10/00B01J4/00
CPCC07C315/00B01J4/004B01J4/007B01J10/00B01J19/0053B01J19/0066B01J19/1862B01J2219/00051B01J2219/00162C07C317/14
Inventor 王宏亮徐文梅胡文俊周航峰吴忠郭付俊李林董工兵
Owner 浙江嘉化新材料有限公司
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