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Synthesis method of sodium picosulfate

A technology of sodium picosulfate and a synthetic method, which is applied in the field of drug preparation, can solve problems such as difficult acquisition of raw materials, complex operation of the synthetic method, and unsuitability for industrial production, and achieve shortened reaction time, high yield, and easy control of the reaction process Effect

Pending Publication Date: 2021-09-07
SHANGHAI GAOZHUN PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0016] The technical problem to be solved in the present invention is that the existing synthetic method is relatively complicated to operate, and the raw materials are not easy to obtain, so it is not suitable for industrial production. The present invention provides a synthetic method of sodium picosulfate, which not only has a simple process route, but also has advantages in terms of industrialization. Many advantages such as simpler operation and higher yield, the intermediate purity produced by this method is very high, and it is easy to obtain sodium picosulfate that meets the requirements of the Pharmacopoeia, so as to solve the defects caused by the prior art

Method used

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  • Synthesis method of sodium picosulfate
  • Synthesis method of sodium picosulfate
  • Synthesis method of sodium picosulfate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0056] The reaction formula of embodiment 1 is as follows:

[0057]

[0058] The compound bisacodyl (200g, 1.0eq) was added to 95% ethanol (1000mL), and under stirring, 3mol / L sodium hydroxide aqueous solution (830mL, 4.5eq) was added dropwise, the temperature was controlled at 30-40°C, and the dropwise addition time was About 2 hours, after the dropwise addition was completed, stir at room temperature for 2 hours, and TLC detected the reaction. After the reaction was complete, half of the liquid (900mL) was evaporated under reduced pressure, and water (800mL, 40v / w) was added to the remaining liquid, and activated carbon (10g , 0.05w / w), after stirring for 30min, suction filtration; under normal temperature stirring, dropwise add 3mol / L hydrochloric acid (480mL) to the filtrate to make pH=5-6, after normal temperature stirring for 30min, filter, and water (1000mL, 5v / w) Rinse the filter cake, and dry the solid under vacuum at 50° C. for 16 hours to obtain a white solid P-...

Embodiment 2

[0062] The reaction formula of embodiment 2 is as follows:

[0063]

[0064] In the middle, the compound bisacodyl (200g, 1.0eq) was added to 95% methanol (1000mL), and under stirring, 3mol / L sodium hydroxide aqueous solution (830mL, 4.5eq) was added dropwise, and the temperature was controlled at 40°C-50°C. The addition time is about 1 hour. After the dropwise addition is completed, stir at room temperature for 1-2 hours. TLC detects the reaction. After the reaction is complete, half of the liquid (900 mL) is evaporated under reduced pressure, and water (800 mL, 40 v / w) is added to the remaining liquid. Put in activated carbon (10g, 0.05w / w), stir for 30min, and then filter with suction; while stirring at room temperature, add 3mol / L sulfuric acid (240mL) dropwise to the filtrate to make the pH = 5-6, and stir for 30min at room temperature, then start to filter with suction , wash the filter cake with water (1000mL, 5v / w), and dry the solid under vacuum at 50°C for 16 hour...

Embodiment 3

[0068] The reaction formula of embodiment 3 is as follows:

[0069]

[0070] In the middle, the compound bisacodyl (200g, 1.0eq) was added to 95% ethanol (1000mL), and under stirring, a 3mol / L potassium hydroxide aqueous solution (830mL, 4.5eq) was added dropwise, the temperature was controlled at 20-30°C, and the The time is about 1 hour. After the dropwise addition is completed, stir at room temperature for 1-2 hours. TLC detects the reaction. After the reaction is complete, half of the liquid (900mL) is evaporated under reduced pressure, and water (800mL, 40v / w) is added to the remaining liquid, and put into Activated carbon (10g, 0.05w / w), after stirring for 30min, suction filtration; under stirring at room temperature, add 3mol / L hydrochloric acid (480mL) dropwise to the filtrate to make pH = 5-6, after stirring at room temperature for 30min, start suction filtration, Rinse the filter cake with water (1000 mL, 5 v / w), and dry the solid under vacuum at 50°C for 16 hours...

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Abstract

The invention discloses a synthesis method of sodium picosulfate, which comprises the following steps of: adding bisacodyl into an organic solvent, adding an alkaline substance for reaction, then adjusting the pH value, and filtering to obtain 4, 4'-(2-pyridylmethyl) bisphenol; adding 4, 4'-(2-pyridylmethyl) bisphenol into a reaction solvent, adding an alkaline substance, and then adding a sulfonation reagent for reaction; after the reaction is finished, quenching, extracting, concentrating and recrystallizing to obtain crude sodium picosulfate; and recrystallizing the crude sodium picosulfate again to obtain qualified sodium picosulfate. The method not only has a simple process route, but also has the advantages of simpler operation, higher yield and the like from the aspect of industrialization. The purity of the intermediate produced by the method is very high, sodium picosulfate meeting the requirements of pharmacopoeia is very easily obtained, and the defects caused by the prior art are overcome.

Description

technical field [0001] The invention relates to the field of medicine preparation, in particular to a synthesis method of sodium picosulfate. Background technique [0002] Sodium Picosulfate (Sodium Picosulfate), also known as Sodium Picosulfate, is a commonly used laxative in clinical practice. , to promote intestinal peristalsis and inhibit water absorption in the intestinal tract, showing catharsis effect; [0003] Sodium picosulfate has a mild catharsis effect, and is suitable for various constipation, postoperative defecation assistance, excretion promotion after contrast medium administration, intestinal content elimination before surgery, pretreatment of large intestine examination (endoscopy), and intestinal content elimination wait; [0004] The chemical name of sodium picosulfate is 4,4'-(pyridin-2-ylmethylene) bisphenyl bissulfate sodium salt monohydrate. The drug was first developed by Italian DeAngeli company and later introduced by Japanese Teijin Pharmaceuti...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D213/30
CPCC07D213/30
Inventor 王江淮李维华刘真豪华岳庭
Owner SHANGHAI GAOZHUN PHARMA CO LTD
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