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P-methylsulfonyltoluene preparation method and equipment

A technology of p-methylsulfonyl and p-toluenesulfonyl chloride, applied in the field of pesticides, can solve the problems of large number of equipment, small output per unit time, long reaction time and the like

Inactive Publication Date: 2020-10-23
内蒙古中高化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The reaction time of this kind of process is long, the output per unit time is small, the number of equipment is large, and the operation is cumbersome. In order to solve this problem, the present invention is hereby proposed

Method used

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  • P-methylsulfonyltoluene preparation method and equipment

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] A preparation method of p-thymphenyltoluene, 70g of sodium sulfite, 90g of sodium bicarbonate, and 250g of water are prepared into an aqueous solution, and 90g of p-toluenesulfonyl chloride is heated up to 70°C, and the above-mentioned aqueous solution and the heated p-toluenesulfonyl chloride are continuously added The first-stage pipeline reactor was reacted for 1.5 hours; 70g of sodium chloroacetate was dissolved in 45g of water to prepare an aqueous solution; the material after the reaction of the sodium chloroacetate aqueous solution and the first-level pipeline reactor was continuously put into the second-level pipeline reactor, at 90°C React for 5 hours. After the reaction is completed, gas-liquid separation is carried out. Hydrochloric acid is added to the liquid to adjust the pH value to 7.5. After the reaction is completed, it is cooled to room temperature, filtered with suction, washed with water, drained, and dried to obtain a white solid which is p-thiampheni...

Embodiment 2

[0033] A preparation method of p-thymphenyl toluene, 90g of sodium sulfite, 60g of sodium bicarbonate, and 350g of water are formulated into an aqueous solution, 100g of p-toluenesulfonyl chloride is heated up to 90°C, and the above-mentioned aqueous solution and the heated p-toluenesulfonyl chloride are continuously added The primary reactor was reacted for 4 hours; 80g of sodium chloroacetate was dissolved in 60g of water to prepare an aqueous solution; the material after the reaction between the aqueous solution of sodium chloroacetate and the primary reactor was continuously put into the secondary reactor, and reacted at 100°C for 5 hours. After the reaction is completed, gas-liquid separation is carried out, and hydrochloric acid is added to the liquid to adjust the pH value to 7. After the reaction is completed, it is cooled to room temperature, filtered with suction, washed with water, and dried by suction, and dried to obtain a white solid which is p-thiamphenicol toluen...

Embodiment 3

[0035] A preparation method of p-thymphenyltoluene, 80g of sodium sulfite, 75g of sodium bicarbonate, and 300g of water are formulated into an aqueous solution, and 97g of p-toluenesulfonyl chloride is heated up to 75°C, and the above-mentioned aqueous solution and the heated p-toluenesulfonyl chloride are continuously added The primary reactor was reacted for 2 hours; 78g of sodium chloroacetate was dissolved in 50g of water to prepare an aqueous solution; the material after the reaction between the aqueous solution of sodium chloroacetate and the primary reactor was continuously put into the secondary reactor, and reacted at 95°C for 5.5 hours After the reaction is completed, gas-liquid separation is carried out, and hydrochloric acid is added to the liquid to adjust the pH value to 8. After the reaction is completed, it is cooled to room temperature, filtered with suction, washed with water, and dried by suction, and dried to obtain a white solid which is p-thiamphenicol tolu...

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Abstract

The invention relates to a p-methylsulfonyltoluene preparation method and equipment. The method comprises the following steps: preparing an aqueous solution from sodium sulfite, sodium bicarbonate andwater, and heating p-toluenesulfonyl chloride to 70-90 DEG C; introducing an aqueous solution of sodium sulfite and sodium bicarbonate and the heated p-toluenesulfonyl chloride into a primary reactorfor reaction; dissolving sodium chloroacetate in water to prepare an aqueous solution, and introducing the material after the first-stage reaction and the sodium chloroacetate aqueous solution into asecond-stage reactor for reaction; after the reaction is finished, carrying out gas-liquid separation, and adding hydrochloric acid into a liquid reaction material to adjust the pH value; cooling thereaction material to room temperature, and carrying out suction filtration, water washing, suction drying and drying to obtain a white solid, namely p-methylsulfonyltoluene; the equipment comprises aprimary reactor, a secondary reactor, a preparation kettle, an intermediate tank, a buffer tank and a sodium chloroacetate preparation kettle. The method is continuous, stable, easy to operate, smallin equipment occupied area and high in automation degree, and the yield in unit time is greatly increased.

Description

technical field [0001] The invention relates to the technical field of pesticides, in particular to a preparation method and equipment for p-thymphenyltoluene. Background technique [0002] p-thiamphenicol toluene is an important organic pharmaceutical raw material. It is light brown powdery crystal, melting point 86~88℃, insoluble in water, soluble in common organic solvents. It is an important intermediate of the new broad-spectrum antibiotic thiamphenicol and thiamphenicol glycinate hydrochloride. Because thiamphenicol and its derivative glycinate hydrochloride have low toxicity and small side effects; long curative effect and good antibacterial effect, the antibacterial activity is more than 6 times stronger than that of chloramphenicol. In foreign countries, it has been widely allowed to be used in immunosuppressive state antibiotics and as food and feed additives, etc., and the demand is increasing year by year. [0003] The existing p-thiamphenicol toluene adopts k...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C315/00C07C317/14
CPCC07C315/00C07C317/14
Inventor 袁源朱宏菲杨华春张云云熊攀
Owner 内蒙古中高化工有限公司