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Method for preparing water-soluble indometacin salt

A technology of indomethacin salt and indomethacin, which is applied in the preparation of water-soluble non-steroidal antipyretic and analgesic drugs, and in the field of preparation of water-soluble indomethacin salt, which can solve the mass loss of methanol or ethanol Large, wasteful, unable to be directly applied, etc., to reduce production costs and environmental pollution, improve product quality and yield, and reduce solvent recovery procedures

Inactive Publication Date: 2015-03-25
HENAN LINGXIAN SCI & TECHN PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In addition, the mother liquor not only contains a large amount of alcohol but also has a large water content, which cannot be used directly, and needs to be recycled after rectification treatment, or directly treated as waste liquid, causing waste and polluting the environment
[0005] Since water-soluble indomethacin is easy to turn yellow in methanol or ethanol, the quality of water-soluble indomethacin produced by this method is poor, and there are a series of problems such as low yield, difficult raw material recovery, and high cost. , especially in the process of centrifugation and solvent recovery, the mass loss of methanol or ethanol is too large, the environmental pollution is serious, and the cost of recycling anhydrous methanol or anhydrous ethanol is high, which does not meet the requirements of the development of green chemistry at home and abroad

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Add 180mL of purified water into a 250mL three-neck flask, start stirring, add 35.8g of indomethacin, adjust the temperature of the reaction system to 60°C, add 8.5g of sodium bicarbonate in batches, adjust the pH value of the reaction solution to 12, and keep at 60°C Stir the reaction for 6 hours to complete the reaction, lower the temperature to 5°C, and continue to stir for 2 hours, filter with suction, and dry the filter cake to obtain water-soluble indomethacin. The yield is 90% based on indomethacin. After high-performance liquid phase analysis, The content is greater than 99.5%, the impurity content is less than 0.1%, and the colorimetry is qualified.

Embodiment 2

[0023] Add 150mL of purified water into a 250mL three-neck flask, start stirring, add 35.8g of indomethacin, adjust the temperature of the reaction system to 75°C, add 3.9g of sodium hydroxide in batches, adjust the pH value of the reaction solution to 14, and keep at 75°C Stir the reaction for 5 hours to complete the reaction, lower the temperature to 10°C, and continue to stir for 2 hours, filter with suction, and dry the filter cake to obtain water-soluble indomethacin. The yield is 85% based on indomethacin. After HPLC analysis, The content is greater than 99.5%, the impurity content is less than 0.1%, and the colorimetry is qualified.

Embodiment 3

[0025] Add 1500L of purified water into a 2000L reactor, start stirring, add 358kg of indomethacin, adjust the temperature of the reaction system to 100°C, add 84kg of sodium bicarbonate in batches, adjust the pH value of the reaction solution to 13, and carry out the stirring reaction at 100°C The reaction was completed in 5 hours, cooled to 10°C, and continued to stir for 2 hours, suction filtered, and the filter cake was dried to obtain water-soluble indomethacin. The yield was 95% based on indomethacin, and the content was greater than 99.5%, the impurity content is less than 0.1%, and the colorimetry is qualified.

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PUM

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Abstract

The invention discloses a method for preparing water-soluble indometacin salt, and solves the problems of solvent residue and complicated post-treatment caused by methanol, ethanol and other organic solvents used in the synthesizing process. The method comprises the following steps: adding an alkaline compound in a mixture of indometacin and water in batches at 0-100 DEG C; controlling the pH value of the solution to 6-14; keeping the temperature of the solution to react the indometacin with the alkaline compound for 2-10 hours in a water solution; crystallizing, filtering, collecting a filter cake and drying to obtain the indometacin salt. The method can be used for simplifying the preparation process and operation steps, greatly improving the product purity and yield and remarkably reducing the production cost and environmental pollution, is environmental friendly, efficient, simple and convenient, and is suitable for industrial production.

Description

technical field [0001] The invention belongs to the field of medicinal chemistry, and in particular relates to a preparation method of a water-soluble non-steroidal antipyretic and analgesic drug, in particular to a preparation method of a water-soluble indomethacin salt. Background technique [0002] Since indomethacin is insoluble in water and difficult to absorb, water-soluble indomethacin sodium or potassium salts are mostly produced and sold as drugs. The water-soluble indomethacin salt is indomethacin sodium or potassium salt. [0003] Indomethacin sodium, also known as 2-methyl-1-(4-chlorobenzoyl)-5-methoxy-1H-indole-3-sodium acetate, molecular formula: C19H15ClNO4Na 3H2O, molecular weight: 433.82, Off-white or slightly yellow crystalline powder, the sodium salt prepared by the reaction of indomethacin and alkaline substances, is a water-soluble non-steroidal antipyretic and analgesic drug. Indomethacin sodium has significant antipyretic, anti-inflammatory, analgesi...

Claims

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Application Information

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IPC IPC(8): C07D209/28
CPCC07D209/28
Inventor 郭有钢贺国超刘裕东刘占领
Owner HENAN LINGXIAN SCI & TECHN PHARMA
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