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Preparation method of water-soluble probenecid salt

A technology of probenecid salt and probenecid, which is applied in the field of chemical synthesis and preparation, can solve the problems of increased cost of organic solvents, difficulty in controlling the amount of residual alkali, and less amount of precipitated solids, so as to reduce energy consumption, complete the reaction efficiently, and produce products The effect of high yield

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

The method for preparing probenecid sodium in this patent has the following disadvantages: a large amount of dehydration and high energy consumption; the cost of using an organic solvent is greatly increased; the anhydrous organic solvent cannot be directly applied after being used once, and can be reused after rectification and anhydrous treatment or It is directly treated as waste liquid; the amount of precipitated solids is small, the yield is low, and the recovery of raw materials is difficult; the biggest problem is that both absolute ethanol and anhydrous acetone have limited solubility to inorganic alkalis, which directly leads to the difficulty in controlling the amount of residual alkali in the resulting product, which is extremely difficult. Earth affects product quality
The method for preparing probenecid salt in this patent has the following disadvantages: the reaction solution is directly evaporated to dryness without refining, and the residual alkali amount of the obtained product is not easy to control, which greatly affects the product quality; the amount of dehydration is large and the energy consumption is high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Add 180mL of pure water into a 500mL three-necked bottle, start stirring, add 28.5g of probenecid, control the system temperature at 100°C, add 15g of liquid caustic soda (32%) dropwise, adjust the pH of the system to 14, and stir for 6 hours to complete the reaction. Cool down to -10°C and continue stirring for 1 hour, filter with suction, and dry the filter cake to obtain water-soluble probenecid. %, the colorimetry is qualified.

Embodiment 2

[0035] Add 150mL of pure water into a 250mL three-necked bottle, start stirring, add 28.5g of probenecid, cool down the system to 10°C, add 12.7g of sodium carbonate in batches, control the rate of addition, ensure that the temperature of the reaction system is at 10-20°C, adjust The pH of the system reached 14, and the reaction was completed by continuing to keep stirring at 20° C. for 6 hours. Cool down to 10°C and continue to stir for 1 hour, filter with suction, and dry the filter cake to obtain water-soluble probenecid. The yield is 85% based on probenecid. According to high-performance liquid chromatography analysis, the content is greater than 99.5%, and the impurity content is less than 0.1%. , the color comparison is qualified.

Embodiment 3

[0037] Add 120mL of pure water into a 250mL three-necked bottle, start stirring, add 28.5g of probenecid, adjust the temperature of the system to 75°C, add 6.5g of sodium methoxide (32%) in batches, adjust the pH of the system to 14, and continue to maintain 75°C Stir for 6 hours and the reaction is complete. Cool down to -10°C and continue to stir for 1 hour, filter with suction, and dry the filter cake to obtain water-soluble probenecid. The yield is 88% based on probenecid. According to high-performance liquid chromatography analysis, the content is greater than 99.5%, and the impurity content is less than 0.1 %, the colorimetry is qualified.

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PUM

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Abstract

The invention discloses a preparation method of a water-soluble probenecid salt. The preparation method comprises the following steps in sequence: reacting probenecid with an alkaline matter in water to obtain the probenecid salt; separating out the probenecid salt from the reaction liquid by controlling the temperature and pH (Potential of Hydrogen) of reaction liquid; and filtering and drying, so as to obtain the probenecid salt. The preparation method is completely carried out under a water phase, no other organic solvents are adopted, no 'three wastes' are brought basically, and the solvent recovery processes are reduced; the production cost and environmental pollution are greatly reduced through the preparation method, and the requirement on clean production is met; the probenecid salt is obtained in a crystallization mode instead of the mode of drying the solvent by distilling, so that other reaction product residues can be avoided, and the production quality and yield of the probenecid salt can be obviously improved.

Description

technical field [0001] The invention relates to a method for preparing water-soluble probenecid salt by using water as a solvent, belonging to the field of chemical synthesis preparation. Background technique [0002] Probenecid, also known as carboxybenzsulfonamide, molecular formula is C 13 h 19 NO 4 S, is a white crystalline powder, soluble in acetone, slightly soluble in ethanol or chloroform, almost insoluble in water, mainly used in the intermission and chronic phase of gout to control hyperuricemia, suitable for increased blood uric acid, renal function It is also used for the treatment of hyperuricemia caused by thiazide diuretics or the risk of gout in patients who are still well and do not excrete much uric acid every day. It is generally not used as an adjuvant treatment for hyperuricemia caused by cancer treatment. Probenecid is insoluble in water and cannot be made into liquid preparations, so its application is limited. Therefore, its water-soluble sodium or...

Claims

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Application Information

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IPC IPC(8): C07C303/40C07C311/16
Inventor 岳涛迟金龙胡波王云超赵景瑞纪晓红魏凤
Owner CHEM TECH ACAD OF SHANDONG PROVINCE
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