Method for preparing high purity sodium picosulfate

A technology of sodium picosulfate and high purity, applied in the field of preparation of high-purity sodium picosulfate, can solve the problems of low yield, high reaction temperature, difficult post-processing, etc., and achieves high purity, simple reaction, and easy post-processing. Effect

Inactive Publication Date: 2013-05-08
SHANDONG INST OF PHARMA IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, when sulfuric acid is carried out with chlorosulfonic acid, there are chlorine atoms on both adjacent positions of the hydroxyl group. Due to the influence of steric hindrance, the reaction temperature is relatively high, reaching 75-80 ° C, and the yield is low, only 40 About % yield
At the same time, a large amount of concentrated sulfuric acid is used as a reaction catalyst and solvent in the reaction process of 2,6-dichlorophenol and 2-pyridine formaldehyde. After the reaction is completed, a very viscous reactant is formed, and the post-treatment is very difficult.

Method used

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  • Method for preparing high purity sodium picosulfate
  • Method for preparing high purity sodium picosulfate
  • Method for preparing high purity sodium picosulfate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Add 81g of bisacodyl to 300ml of water to form a suspension solution, then add 380ml of water and 39g of sodium hydroxide to prepare an alkaline solution, and when the mixture is heated to 50°C, the bisacodyl will be completely dissolved, and the reaction will be maintained at 50°C for 40 minutes After cooling to room temperature, 300 ml of 10% dilute hydrochloric acid was added to precipitate a solid. Filter, wash with water, and dry the solid under reduced pressure and constant temperature at 80°C to obtain 58.8 g of 4,4'-dihydroxyphenyl-(2-pyridine)methane.

Embodiment 2

[0033] Add 81g of bisacodyl to 300ml of water to form a suspension solution, then add 380ml of water and 39g of sodium hydroxide to prepare an alkaline solution, heat the mixture to 70°C and keep stirring at this temperature for 30 minutes, cool to room temperature, add 10% dilute hydrochloric acid 300ml, precipitated solid. Filter, wash with water, and dry the solid under reduced pressure and constant temperature at 80°C to obtain 57.6g of 4,4'-dihydroxyphenyl-(2-pyridine)methane.

Embodiment 3

[0035] Add 81g of bisacodyl into 300ml of water to form a suspension solution, then add 380ml of water and 54.7g of potassium hydroxide to prepare an alkali solution, and when the mixture is heated to 50°C, the bisacodyl can be completely dissolved, and the reaction is maintained at 50°C with stirring After 40 minutes, it was cooled to room temperature, and 220 ml of 25% dilute sulfuric acid was added to precipitate a solid. Filter, wash with water, and dry the solid under reduced pressure and constant temperature at 80°C to obtain 58.2 g of 4,4'-dihydroxyphenyl-(2-pyridine)methane.

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Abstract

The invention relates to a method for preparing high purity sodium picosulfate. The method is characterized in that based on bisacodyl as the starting material, sodium picosulfate is prepared by hydrolysis reaction and sulphating reaction. The preparation method is simple in process flow, simple and convenient to operate, and suitable for industrial production. The sodium picosulfate prepared is high in purity and meets the quality standard required by European and United States Pharmacopeia.

Description

technical field [0001] The invention relates to a preparation method of sodium picosulfate. Specifically relate to the preparation method of high-purity sodium picosulfate. Background technique [0002] Constipation refers to a decrease in the number of stools, generally less than 3 times a week, accompanied by difficulty in defecation and dry stool. Constipation is a common clinical symptom. It persists for a long time. The symptoms are disturbing and affect the quality of life. There are various etiologies, and intestinal diseases are the most common. Constipation not only reduces the quality of life of patients, but is also closely related to the occurrence of diseases such as colon cancer, breast disease, and Alzheimer's disease. Severe cases can cause cardiovascular and cerebrovascular accidents. Therefore, early prevention and reasonable treatment can reduce the serious consequences of constipation. [0003] Sodium picosulfate (chemical name: 4,4'-(pyridin-2-ylmethyl...

Claims

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Application Information

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IPC IPC(8): C07D213/30
Inventor林振广刘宜辉曹冲
OwnerSHANDONG INST OF PHARMA IND