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Probenecid purification method

A purification method, technology of probenecid, applied in chemical instruments and methods, organic chemistry, preparation of organic compounds, etc., can solve problems such as hazards to environmental operation workers, difficulty in product recycling, and many processes, so as to reduce production costs and Environmental pollution, significant economic and social benefits, and the effect of simplifying the process of operation

Active Publication Date: 2013-03-20
CHEM TECH ACAD OF SHANDONG PROVINCE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, alcohol elution is mainly used to purify probenecid at home and abroad. Because probenecid is easy to turn yellow in ethanol, activated carbon must be added to decolorize by thermal filtration, and alcohol washing can only obtain a product with a purity of 98%. There is still a big gap between the standards stipulated in the pharmacopoeias of various countries, so it must go through two times of alcohol elution to obtain qualified products
The main problem of this method is that the amount of ethanol is large, and the feeding ratio of each decolorization crystal is probenecid: absolute ethanol=1:8 (w / w)
The use of a large amount of volatile organic solvents will inevitably cause a large amount of volatilization loss of organic solvents in the process of centrifugation and solvent recovery, which will cause great harm to the environment and operators
It is difficult or impossible to recover the products remaining in a large amount of organic solvents, so that the recovery rate of probenecid refining is only about 73%
This purification method not only has many procedures and a long cycle, but also has low yield, high cost and a lot of waste.
This method does not meet the requirements of developing green low-carbon chemistry and promoting clean production at home and abroad, so a new technology is urgently needed to solve the existing problems and meet market demand

Method used

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  • Probenecid purification method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Add 100 mL of pure water into a 250 ml three-necked flask, start stirring, add 28.5 g of crude probenecid, heat to 50-60°C, add 12.1 g of dipropylamine dropwise, and continue stirring at 50-60°C for 2 hours. Then the temperature was lowered to -20°C, and stirring was continued at -20°C for 4 hours.

[0031] Filter, add the filter cake to 80 mL of pure water, heat to 50-60°C, stir for 1 hour to dissolve it all. Add hydrochloric acid (31%) dropwise into the system to adjust p H=1-2, continue to stir for 1 hour, retest p When H is 1-2, the acidification is completed.

[0032] Filtrate, add the filter cake to 180 mL of pure water, heat to 30-40°C, stir and wash with water for 1 hour, filter while hot, and dry to obtain the finished product of probenecid. The yield is 92% based on the crude product of probenecid. High-performance liquid chromatography analysis, the content is greater than 99%, and the impurity content is less than 0.1%.

Embodiment 2

[0034] Add 100 mL of pure water into a 250 ml three-necked flask, start stirring, add 28.5 g of crude probenecid, heat to 50-60°C, add 5.4 g of dimethylamine dropwise, and continue stirring at 50-60°C for 2 hours. Then the temperature was lowered to -10°C, and stirring was continued at -10°C for 4 hours.

[0035] Filter, add the filter cake to 80 mL of pure water, heat to 50-60°C, stir for 1 hour to dissolve it all. Add hydrochloric acid (31%) dropwise into the system to adjust p H=1-2, continue to stir for 1 hour, retest p When H is 1-2, the acidification is completed.

[0036] Filtrate, add the filter cake to 180 mL of pure water, heat to 30-40°C, stir and wash with water for 1 hour, filter while hot, and dry to obtain the finished product of probenecid. The yield is 87% based on the crude product of probenecid. High-performance liquid chromatography analysis, the content is greater than 99%, and the impurity content is less than 0.1%.

Embodiment 3

[0038] Add 80 mL of pure water into a 250 ml three-necked flask, start stirring, add 28.5 g of crude probenecid, heat to 20-30°C, add 13.8 g of sodium hydroxide aqueous solution (32%) dropwise, and keep at 20-30°C Stir for 1 hour. Then the temperature was lowered to -20°C, and stirring was continued at -20°C for 6 hours.

[0039]Filter, add the filter cake to 80 mL of pure water, heat to 20-30°C, and stir for 1 hour to dissolve it completely. Add hydrochloric acid (31%) dropwise into the system to adjust p H=1-2, continue to stir for 1 hour, retest p When H is 1-2, the acidification is completed.

[0040] Filtrate, add the filter cake to 180 mL of pure water, heat to 30-40°C, stir and wash with water for 1 hour, filter while hot, and dry to obtain the finished product of probenecid. The yield is 90% based on the crude product of probenecid. High-performance liquid chromatography analysis, the content is greater than 99%, and the impurity content is less than 0.1%.

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Abstract

The invention discloses a probenecid purification method, comprising the steps of: reacting a crude probenecid product and an alkaline substance in water until the probenecid is dissolved completely; cooling an obtained solution to carry out low-temperature crystallization, and stirring till complete crystallization; filtering, dissolving the obtained filter cakes with water, and then, adding acid to regulate the obtained solution to be acidic; and filtering, washing the obtained filter cakes with water, and then filtering and drying to obtain a pure probenecid product. According to the invention, by utilization of chemical principles of crystallization and filtration, the purpose of purifying the probenecid in a water environment is achieved by alkaline dissolution and acidification operation. The probenecid purification method is simple to operate and free from utilization of organic solvents, so that the production cost and environment pollution are reduced greatly, and the requirement for clean production is met.

Description

technical field [0001] The invention relates to a method for purifying probenecid, which belongs to the field of chemical synthesis preparation. Background technique [0002] p-(Dipropylaminosulfonyl)benzoic acid (referred to as probenecid), English name 4-[(Dipropylamino)sulfonyl]benzoic acid, CAS number: 57-66-9, molecular formula: C 13 h 19 NO 4 S, molecular weight: 285.36, melting point 194-196°C. Probenecid is white crystal, odorless, slightly bitter taste, soluble in acetone, soluble in dilute sodium hydroxide solution, slightly soluble in ethanol or chloroform, almost insoluble in water and dilute acid, mainly in the inter-aggressive and chronic phase of gout It is used to control hyperuricemia. It is suitable for patients with increased blood uric acid, good renal function, and little uric acid excretion every day. It is also used for the treatment of hyperuricemia caused by thiazide diuretics or the risk of gout. Not as an adjuvant treatment for hyperuricemia du...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C311/16C07C303/44
Inventor 王云超李培培游淇岳涛赵景瑞柳泽岳
Owner CHEM TECH ACAD OF SHANDONG PROVINCE
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