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Industrial production method of s-(-)-ornidazole disodium phosphate

A technology of levo-ornidazole and crude product of levo-ornidazole, applied in the field of disodium phosphate of levo-ornidazole, can solve problems affecting product quality, high boiling point, residue, etc., to achieve environmental protection, improve product quality, The effect of lowering the limit

Inactive Publication Date: 2015-01-28
YANGTZE RIVER PHARM GRP NANJING HAILING PHARM CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

According to the ICH classification, toluene belongs to Class II restricted solvent, which is highly toxic and has a high boiling point, making it difficult to remove
Using toluene for recrystallization may result in a certain amount of toluene remaining in the final product, thus affecting product quality

Method used

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  • Industrial production method of s-(-)-ornidazole disodium phosphate
  • Industrial production method of s-(-)-ornidazole disodium phosphate
  • Industrial production method of s-(-)-ornidazole disodium phosphate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] The preparation of embodiment 1 L-ornidazole

[0029] Add 800ml of water to 100g of levorotatory crude product, slowly add dilute hydrochloric acid dropwise to pH 3.0, filter to remove insoluble matter, add saturated sodium bicarbonate solution to the obtained filtrate, adjust pH to 7.5, add about 100mg of saturated sodium chloride solution, A large amount of precipitates precipitated, stirred for about 1-3 hours, filtered, washed with an appropriate amount of water, and dried to obtain 85 g of L-ornidazole with a HPLC purity of 99.8%.

Embodiment 2

[0030] The preparation of embodiment 2 L-ornidazole

[0031] Add 100 g of the crude product of L-ornidazole, add 500 ml of toluene, heat up to 80-100° C. to dissolve and clarify, filter, and the filtrate is slowly cooled to room temperature, crystals are precipitated, filtered, and dried to obtain 80 g of L-ornidazole with an HPLC purity of 99.0%.

Embodiment 3

[0032] The preparation of embodiment 3 L-ornidazole phosphate disodium

[0033] Add 100 g of L-ornidazole, add 600 ml of ethyl acetate, slowly dropwise add 120 ml of phosphorus oxychloride, stir and react at 30°C, after the reaction is completed, concentrate under reduced pressure to remove the solvent to obtain a slurry, add 100 ml of water to the obtained slurry, Adjust the pH to 4 with sodium carbonate, concentrate under reduced pressure, add 200 ml of ethanol to the concentrate, cool to room temperature, filter to remove insoluble inorganic salts, adjust the pH of the obtained filtrate to 7.5 with 20% sodium hydroxide solution, precipitate a white solid, filter, and dry at 30 121 g of L-ornidazole phosphate was obtained by vacuum drying at ℃, the content was 99.5%, and the total inorganic salt content was about 0.16%.

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Abstract

The invention relates to a preparation method of s-(-)-ornidazole disodium phosphate suitable for industrialization. Through the adoption of the scheme, the solvent of methylbenzene in the recrystallization process of S-ornidazole is prevented from being used, and a recrystallization scheme completely without pollution is adopted. Moreover, excess phosphorus oxychloride is removed in advance in the preparation process of the s-(-)-ornidazole disodium phosphate, and thus the content of inorganic salt in a prepared sample is obviously reduced, and the product quality is obviously improved.

Description

technical field [0001] The invention relates to an industrial production method of levo-ornidazole phosphate disodium. Background technique [0002] Phosphorylation is a common prodrug design method, which can improve the water solubility of the parent drug, improve pharmacokinetic properties, improve targeting, reduce drug side effects, increase drug stability, etc., in modern drug development It has been widely valued and applied. [0003] Levo-ornidazole disodium phosphate (I) is a compound with a novel structure developed based on this principle. As a prodrug of levo-ornidazole, this product has significant clinical advantages over ornidazole. In recent years, It is in the stage of clinical research and has the potential to be used in clinical practice as a new generation of antibacterial drugs. [0004] [0005] Chinese patent CN200610166893.2 discloses L-ornidazole ester and its application in anti-anaerobic bacteria and protomicrobial infection, and briefly expla...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/6506
Inventor 王先登卢翔邓飞黄丁菲张明明刘淑敏
Owner YANGTZE RIVER PHARM GRP NANJING HAILING PHARM CO LTD
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