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Preparation method of azithromycin monohydrate crystal

A technology for azithromycin and monohydrate, which is applied in the field of preparation of azithromycin monohydrate crystals, can solve the problems of inability to accurately control, cumbersome and difficult to operate, low azithromycin monohydrate content, etc., and achieves convenient operation, small residual solvent content, and moisture absorption. low sex effect

Active Publication Date: 2009-06-03
YICHANG HEC CHANGJIANG PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method is loaded down with trivial details not easy to operate, can't control the operation when distilling organic solvent accurately, the content of the azithromycin monohydrate that obtains is not high

Method used

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  • Preparation method of azithromycin monohydrate crystal
  • Preparation method of azithromycin monohydrate crystal
  • Preparation method of azithromycin monohydrate crystal

Examples

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preparation example Construction

[0028] The invention discloses a method for preparing crystals of azithromycin monohydrate, which comprises the following steps:

[0029] (1) Sample dissolution: dissolve the crude product of azithromycin in anhydrous methanol to obtain solution I;

[0030] (2) Crystallization: take solution I and press filter to remove insoluble matter to obtain solution II, add pure water dropwise to solution II while stirring, after the crystallization of azithromycin, centrifuge to collect the wet product of azithromycin;

[0031] (3) Pulverization: pulverize the azithromycin wet product obtained in step (2) into 60-100 meshes;

[0032] (4) Water exchange: add pure water to the pulverized azithromycin wet product obtained in step (3), and stir for 8 to 10 hours to obtain a suspension;

[0033] (5) Drying: the suspension is centrifuged to collect azithromycin crystals and dried to constant weight to obtain azithromycin monohydrate crystals.

[0034] Step (1) is carried out at 40-50°C.

...

Embodiment 1

[0049] Preheat 35kg of anhydrous methanol to 40°C, add 7kg of azithromycin, heat to 45°C, and keep warm for 1 hour. Filter to remove insoluble impurities to obtain azithromycin-methanol solution. Cool the solution to 40°C, stir quickly, add 11kg of pure water dropwise within 1 hour, keep the solution temperature at 40°C, continue to stir, and after growing the crystal for 1.5 hours, continue to add 24kg of pure water dropwise, and control it within 2 hours After the addition, continue to stir until crystallization, and grow crystals for 1.5 hours. Cool down to 23°C and keep warm for 1 hour. Filter to obtain azithromycin wet product, crush the azithromycin wet product into 60 mesh, add 70kg of pure water, stir for 8 hours, centrifuge, wash the azithromycin wet product twice with pure water, and continue to centrifuge for 5 minutes. Dry the wet product of azithromycin in a vacuum drying oven at 45°C to constant weight to obtain off-white powder, which is the crystal of azithro...

Embodiment 2

[0051]Preheat 28kg of anhydrous methanol to 40°C, add 1kg of azithromycin, heat to 50°C, and keep warm for 0.5 hours. Filter to remove insoluble impurities to obtain azithromycin-methanol solution. Cool the solution to 42°C, stir quickly, add 11kg of pure water dropwise within 1.5 hours, keep the solution temperature at 40°C, continue to stir, and after 1.5 hours of crystal growth, continue to drop 24kg of pure water within 1.5 hours After the addition, continue to stir until crystallization, and grow crystals for 1.5 hours. Cool down to 25°C and keep warm for 1 hour. Filter to obtain azithromycin wet product, crush the azithromycin wet product into 80 mesh, add 10kg of pure water, stir for 10 hours, centrifuge, wash the azithromycin wet product twice with pure water, and continue centrifuging for 5 minutes. Dry the wet product of azithromycin in a vacuum drying oven at 25°C to constant weight to obtain off-white powder, namely azithromycin monohydrate crystals, with azithro...

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Abstract

The invention provides a preparation method of an azithromycin monohydrate crystal. The preparation method comprises the following steps: (1) dissolving a sample; (2) crystallizing; (3) pulverizing; (4) performing water exchange; and (5) drying. The azithromycin monohydrate crystal prepared by the method has the advantages of low hygroscopicity, 4-6.5% water content, less solvent residue, almost no degradation after long-time standing, good stability and stable infrared ray and X-ray characteristics, and all indexes conform to test standards of United States Pharmacopeia (usp31).

Description

technical field [0001] The invention relates to the field of azithromycin, in particular to a preparation method of azithromycin monohydrate crystals. Background technique [0002] Azithromycin (chemical name: 9-deoxy-9a-aza-9a-methyl-9a-homoerythromycin A) is derived from erythromycin A and is used to treat diseases such as bronchial infection, sexual contact infection and skin infection The semi-synthetic macrolide antibiotics, its chemical structural formula is as follows: [0003] [0004] U.S. Patent No. 4,517,359 first disclosed azithromycin and its preparation method. It disclosed that 9-deoxy-9-deoxy-9a-aza-9a-9a-homoerythromycin A was produced in halogenated hydrocarbons in the presence of excess formaldehyde and formic acid. Such as chloroform or carbon tetrachloride as a solvent for the methylation reaction to obtain azithromycin. [0005] Azithromycin exists in three forms, anhydrous, monohydrate and dihydrate. US Patent No. 4,517,359 discloses anhydrous az...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H17/08A61P31/04
Inventor 卢轩符兆林尹建湘
Owner YICHANG HEC CHANGJIANG PHARMA CO LTD
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