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Synthesis and preparation method for probenecid sodium and probenecid potassium

A technology of probenecid sodium and probenecid potassium, which is applied in the preparation of sulfonic acid amide, organic chemistry and other directions, can solve the problems of less probenecid sodium and unsatisfactory results, and achieve the effect of easy process means

Inactive Publication Date: 2013-02-13
BEIJING KANGZHENG KANGREN BIOTECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

After testing, when ethanol (95%) is used as the solvent, although the water content is not large, after the reaction is terminated, the crystals of probenecid sodium (potassium) are still less, and the crystallization yield after concentration is about 50%. The result is not ideal

Method used

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  • Synthesis and preparation method for probenecid sodium and probenecid potassium

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] 1, the synthesis of probenecid sodium

[0014] 1.1 Reaction material

[0015] Probenecid 100g

[0016] Absolute ethanol 1 500ml (for dissolving probenecid)

[0017] Sodium hydroxide 14g

[0018] Absolute ethanol 2 350ml (for dissolving sodium hydroxide)

[0019] 1.2 The process method is as follows:

[0020] Put a 2000ml three-necked flask with stirring, reflux condensing device and dropping funnel in a water bath, add probenecid and anhydrous ethanol in which probenecid is dissolved, start stirring, heat the water bath to 75-80°C, and keep this temperature, After the probenecid is completely dissolved, add the sodium hydroxide anhydrous ethanol solution that has been dissolved in advance at 70°C dropwise at a rate of about 5ml per minute, and continue to react for 15 minutes after dropping, then slightly lower the temperature to 50-60°C, and reflux to condense The tube is changed to a distillation condenser, and the temperature of the water bath is raised to 90-95...

Embodiment 2

[0036] 1, the synthesis of probenecid potassium

[0037] 1.1 Reaction material

[0038] Probenecid 100g

[0039] Absolute ethanol 1 500ml (for dissolving probenecid)

[0040] Potassium hydroxide 19.65g

[0041] 2 500ml absolute ethanol (for dissolving potassium hydroxide)

[0042] 1.2 The process method is as follows

[0043] Put a 2000ml three-necked flask with stirring, reflux condensing device and dropping funnel in a water bath, add probenecid and anhydrous ethanol in which probenecid is dissolved, start stirring, heat the water bath to 75-80°C, and keep this temperature, After the probenecid is completely dissolved, add the potassium hydroxide anhydrous ethanol solution that has been dissolved in advance at 70°C dropwise at a rate of about 5ml per minute, continue the reaction for 15 minutes after dropping, cool down slightly to 50-60°C, and reflux to condense The tube is changed to a distillation condenser tube, the water bath is heated to 90-95°C, concentrated, con...

Embodiment 3

[0059] 1, the synthesis of probenecid sodium

[0060] 1.1 Reaction material

[0061] Probenecid 1g

[0062] Absolute ethanol 1 5ml (for dissolving probenecid)

[0063] Sodium hydroxide 0.14g

[0064] Absolute ethanol 2 3.5ml (for dissolving sodium hydroxide)

[0065] 1.2 The process method is as follows:

[0066] Put a 2000ml three-necked flask with stirring, reflux condensing device and dropping funnel in a water bath, add probenecid and anhydrous ethanol in which probenecid is dissolved, start stirring, heat the water bath to 75-80°C, and keep this temperature, After the probenecid is completely dissolved, add the sodium hydroxide anhydrous ethanol solution that has been dissolved in advance at 70°C dropwise at a rate of about 5ml per minute, and continue to react for 15 minutes after dropping, then slightly lower the temperature to 50-60°C, and reflux to condense The tube is changed to a distillation condenser, and the temperature of the water bath is raised to 90-95°C...

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Abstract

The invention relates to a synthesis and preparation method for probenecid sodium and probenecid potassium. The method is characterized by comprising the following steps: heating water bath to reach 75 to 80 DEG C to completely dissolve probenecid in absolute ethyl alcohol; then dropping a mixed solution of sodium hydroxide or potassium hydroxide or absolute ethyl alcohol which is dissolved in advance at 70 DEG C at speed of 5ml per minute; further reacting for 15 minutes after dropping; slowly cooling to reach 50 to 60 DEG C; replacing a reflux condensing pipe by a distilling condensing pipe; heating the water bath to reach 90 to 95 DEG C; condensing until the volume is 1 / 5 of original volume; pouring out the reactant while hot; standing for more than 4 hours at cold condition; leaching to obtain rough products of probenecid sodium and probenecid potassium; and further refining to obtain the products probenecid sodium and probenecid potassium. According to the synthesis and preparation method, the absolute ethyl alcohol is adopted as the solvent, so that more crystals are separated after cooling when the reaction is finished, and the yield can reach over 80% after condensing; and the technical means for purifying and recrystallizing the probenecid sodium (potassium) is easy to operate, and suitable for industrial production.

Description

technical field [0001] The invention relates to a synthesis and preparation method of probenecid sodium and probenecid potassium, which is applicable to the pharmaceutical field. Background technique [0002] It is well known that probenecid, in addition to its role in the treatment of chronic gout, can significantly optimize the pharmacokinetic properties of various β-lactam antibiotics. At present, a compound preparation composed of probenecid and ampicillin has been used clinically. The combined application of probenecid and various β-lactam antibiotics can not only greatly reduce the dosage of corresponding antibiotics, thereby reducing the incidence of adverse reactions to antibiotics, but also increase the compliance of antibiotic treatment and reduce the risk of drug resistance. Selection of medicinal bacteria. [0003] Because probenecid is almost insoluble in water, when it is combined with penicillins for injection to form compound injections, it is necessary to ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C311/16C07C303/40
Inventor 吴晓辉
Owner BEIJING KANGZHENG KANGREN BIOTECH
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