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
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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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