Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

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
View PDF3 Cites 1 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Synthesis method of 1-methyl-4-methyl sulfonyl benzene

Examples

Experimental program
Comparison scheme
Effect test

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-...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

The invention discloses a synthesis method of 1-methyl-4-methyl sulfonyl benzene. The synthesis method comprises the following steps: stirring 4-methylbenzene sodium sulfinate and chloromethane for four stages of methylation, so as to obtain a 1-methyl-4-methyl sulfonyl benzene mixed solution, putting the mixed solution into a liquid separation tower for stewing separation, and then carrying out washing, crystallization and dewatering to obtain a 1-methyl-4-methyl sulfonyl benzene product. According to the synthesis method, through the adoption of self-sucking stirring, a stirrer rotates in liquid to generate negative pressure, and under the condition of the negative pressure, chloromethane gas is sucked to enhance gas-liquid contact reaction to complete the reaction; furthermore, pressures on the surfaces of four methylation kettles are kept to be equal, so that liquid in the kettles full overflows; due to the adoption of the single-stage liquid separation tower, material blockage isprevented; continuous production is realized.

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

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Applications(China)
IPC IPC(8): C07C315/00C07C317/14B01J19/18B01J10/00B01J4/00
CPCB01J4/004B01J4/007B01J10/00B01J19/0053B01J19/0066B01J19/1862C07C315/00B01J2219/00162B01J2219/00051C07C317/14
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
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com