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Production process of methyl p-tolyl sulfone

A technology of methylsulfonyl toluene and p-methylsulfonyl toluene, which is applied in the field of production technology of p-methylsulfonyl toluene, can solve the problems of high production cost, high toxicity of dimethyl sulfate, long cycle and the like, and achieves reduction of production cost and cycle time. , reduce the risk of environmental pollution, and facilitate the effect of safe production

Inactive Publication Date: 2009-05-20
ANJI HAOSEN PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] The traditional three-step reaction method has high production costs and a long cycle, especially the final crystallization section, which takes 30 hours; in addition, the dimethyl sulfate used in the reaction is highly toxic and explosive, polluting the environment, and the production environment is poor

Method used

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  • Production process of methyl p-tolyl sulfone
  • Production process of methyl p-tolyl sulfone
  • Production process of methyl p-tolyl sulfone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Add 1800kg of water, 700kg of p-methylsulfonesulfonyl chloride, 450kg of sodium bicarbonate and 330kg of sodium sulfite to the salt-forming kettle, and carry out a salt-forming reaction under normal pressure, with a reaction temperature of 60°C and a holding time of 4 hours. The carbon dioxide gas produced by the reaction and a small amount of After the reaction is completed, filter at 40-50°C while it is still hot. The mother liquor is pumped into the methylation kettle by vacuum, and the filter residue is treated separately. The mother liquor is further heated to 70°C in the methylation tank at 0.5kg / cm 3 Under pressure, pass 158kg of monochloromethane gas, keep warm and cool to crystallize. When the crystallization mother liquor is cooled to 40°C, it is discharged and filtered, and the filter cake is centrifuged by a centrifuge. The filtered mother liquor and the centrifuged mother liquor are concentrated and distilled. The water vapor is condensed by the condenser a...

Embodiment 2

[0027] Add 1700kg of water, 720kg of p-methylsulfonesulfonyl chloride, 450kg of sodium bicarbonate and 300kg of sodium sulfite to the salt-forming kettle to perform a salt-forming reaction under normal pressure. The reaction temperature is 60°C and the holding time is 3 hours. The carbon dioxide gas and a small amount of water produced by the reaction Empty, after the reaction is completed, filter at 45°C while it is still hot, vacuum pump the mother liquor into the methylation kettle, and process the filter residue separately. The mother liquor is further heated to 85°C in the methylation tank at 0.4kg / cm 3 Under pressure, pass 140kg of monochloromethane gas, keep warm and cool to crystallize. When the crystallization mother liquor is cooled to 40°C, it is discharged and filtered, and the filter cake is centrifuged by a centrifuge. The filtered mother liquor and the centrifuged mother liquor are concentrated and distilled. The water vapor is condensed by the condenser and use...

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Abstract

The invention relates to a manufacturing technology of pharmaceutical intermediates, in particular to a manufacturing technology of P-methylsulfonyl toluene. The invention provides a manufacturing technology of the P-methylsulfonyl toluene, which includes the following steps: (1) the salt-forming reaction of P-methylsulfonyl sulfonic acid chloride; and (2) the methylation reaction of P- toluene sodium sulfinate generated in step (1), wherein step (2) is that P-methylsulfonyl sulfonic acid chloride reacts with monochloro methane to generate the P-methylsulfonyl toluene which is shown as a reaction formula (c). Compared with the conventional technology, the technology has two very distinct advantages: firstly, a two-step reaction method replaces the conventional three-step reaction method so as to greatly reduce the production costs and cycle; and secondly, monochloro methane with low toxicity replaces explosive dimethyl sulfate with high toxicity, thereby not only reducing the risk of environmental pollution and being more in line with the requirements of environmental protection, but also greatly improving labor conditions and being more conducive to safe production.

Description

technical field [0001] The invention relates to a production process of a pharmaceutical intermediate, in particular to a production process of p-thiamphenicol toluene. Background technique [0002] P-thiamphenicol toluene is the main raw material for producing p-thiamphenicol phenylserine ethyl ester, and p-thiamphenicol phenylserine ethyl ester is the main raw material for producing thiamphenicol and fluprofen. Fluprofen and thiamphenicol are national second-class new drugs, and they are also products that are encouraged to be developed by the state. Fluprofen is a broad-spectrum veterinary antibiotic developed and developed by the American Shilling Company. It is widely used to kill various "Gram" negative-positive bacteria. It is currently one of the best antibiotics in the world. substitutes for. [0003] Judging from the current situation, the situation of p-thiamphenicol is very good, firstly because p-thiamphenicol is the necessary raw material for the production o...

Claims

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Application Information

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IPC IPC(8): C07C317/14C07C315/04
Inventor 何成红
Owner ANJI HAOSEN PHARMA
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