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Technique for preparing potassium sodium dehydroandroandrographolide succinate

A technology of andrographolide and succinic acid, which is applied in the direction of antipyretics, organic chemistry, non-central analgesics, etc., can solve the problems of unstable pH value, low yield, and low content of the preparation, and achieve less impurities and higher yield. The effect of high efficiency and high product purity

Active Publication Date: 2008-09-10
CHANGCHUN MAILING BIOLOGICAL ENG CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The invention provides a preparation process of potassium half-ester andrographolide succinate sodium salt, which solves the problems of low product yield, low content and unstable pH value of the prepared preparation in the existing preparation process

Method used

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  • Technique for preparing potassium sodium dehydroandroandrographolide succinate
  • Technique for preparing potassium sodium dehydroandroandrographolide succinate
  • Technique for preparing potassium sodium dehydroandroandrographolide succinate

Examples

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Embodiment 1

[0139] Dissolve 200 g of dehydrated andrographolide succinate half ester in 600 ml of absolute ethanol in a 70° C. water bath. 37.6gKHCO 3 with 31.6g NaHCO 3 Add water and dissolve in a 70°C water bath. Slowly add dropwise under stirring at 50°C until the solution is clear, filter, pass through a 0.22μm membrane, then add 1400ml of absolute ethanol, stir evenly while adding, and let it stand at room temperature for 15 hours, and crystallization will occur naturally. Filter, wash twice with 1200ml of absolute ethanol, filter, and dry under reduced pressure at 60°C to obtain 180g of light yellow powder.

Embodiment 2

[0141] 350 g of dehydrated andrographolide succinic acid half ester was dissolved in 1400 ml of absolute ethanol in a 75° C. water bath. 65.8gKHCO 3 with 55.3g NaHCO 3 Add water and dissolve in a 75°C water bath. Slowly add dropwise under stirring at 65°C until the solution is clear, filter, pass through a 0.22μm membrane, then add 3150ml of absolute ethanol, stir evenly while adding, stand at room temperature for 18 hours, and crystallize naturally. Filter, wash 3 times with 2100ml of absolute ethanol, filter, and dry under reduced pressure at 60°C to obtain 292g of light yellow powder.

Embodiment 3

[0143] Dissolve 500 g of dehydrated andrographolide succinate half ester in 3000 ml of absolute ethanol in a water bath at 80°C. 92gKHCO 3 with 78.9g NaHCO 3 Add water and dissolve in 80°C water bath. Slowly add dropwise under stirring at 80°C until the solution is clear, filter, pass through a 0.22μm membrane, then add 5500ml of absolute ethanol, stir evenly while adding, stand at room temperature for 20 hours, and crystallize naturally. Filter, wash 3 times with 3000ml of absolute ethanol, filter, and dry under reduced pressure at 60°C to obtain 445g of light yellow powder.

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Abstract

The invention discloses a process of preparing Dehydroandrographolide Succinate Sodium and Potassium salts. The process includes: heating and dissolving Dehydroandrographolide Succinate with 3 to 6 times of absolute ethyl alcohol; adding mole KHCO3 and NaHCO3 in equal weight into water and dissolving in a water bath; dripping slowly while mixing in the temperature of between 50 and 80 DEG C until solution defecates, filtering and putting on a 0.22 mu m filter membrane, adding 7 to 11 times of absolute ethyl alcohol while mixing until the solution is even, standing in room temperature until natural crystallization seeds out, filtering and washing 2 to 3 times with absolute ethyl alcohol, fitering and drying with less pressure to obtain a canary solid. The invention provides a process route of preparing potassium sodium dehydroandroan drographolide succinate for injection with high purity, which uses Dehydroandrographolide Succinate as the raw material, is added with potassium bicarbonate and sodium bicarbonate directly to compose Potassium Sodium Dehydroandroan drographolide Succinate, which is high in process yields, high in product purity, good in solubility, less in impurity and complete in combination of Potassium and Sodium; the product is high in purity and good in solubility without obvious toxic and side effect in clinic application, the preparation is more stable compared with the similar and can be prepared into various preparations.

Description

technical field [0001] The invention discloses a preparation process of potassium half ester succinate sodium salt of andrographolide, which is an optimization and improvement of the existing production process and belongs to the technical field of chemical medicine preparation. Background technique: [0002] The present invention relates to dehydroandrographolide potassium half ester succinate sodium salt (common name: Yanhuning), chemical name is: 14-dehydroxyl-11,12-didehydroandrographolide-3,19-di Potassium succinate half ester sodium salt, the main structure is dehydroandrographolide succinate half ester, which has the functions of clearing heat, antibacterial, anti-inflammatory, and antiviral; the current traditional technology is to use chuanhuning and sodium bicarbonate as raw materials, and acid-base reaction in water And reaction, through sterile filtration, Yanhuning was prepared under freeze-drying conditions, the product yield was low, the content was not high, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/58A61P29/00A61P31/12
Inventor 杜宏明高强苏中孙玉芹
Owner CHANGCHUN MAILING BIOLOGICAL ENG CO LTD
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