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Roxithromycin refining method

A technology of roxithromycin and refining method, applied in chemical instruments and methods, preparation of sugar derivatives, sugar derivatives, etc., can solve the problems affecting the stability and efficacy of roxithromycin, the comprehensive removal rate of impurities is not high, Problems such as low product quality and yield, to achieve the effect of good impurity removal effect, good appearance and color, and high product yield

Inactive Publication Date: 2014-11-26
ZHENGZHOU HOUYI PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0017] The content of these impurities in crude roxithromycin reaches more than 3%, which seriously affects the stability and efficacy of roxithromycin
The refining method of existing roxithromycin is to adopt organic solvent or the mixed solvent of organic solvent and water, crude roxithromycin is purified, generally only for one or two kinds of impurities in the crude roxithromycin, and The comprehensive removal rate of all impurities is not high, and the quality yield of the product is also low; at the same time, most of the existing methods are complicated in process and long in process, which are not suitable for popularization and application

Method used

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Embodiment 1

[0034] The refining method of the roxithromycin of the present embodiment may further comprise the steps:

[0035] 1) Disperse 100g of crude roxithromycin in a mixed solvent formed by mixing 50ml of methanol and 50ml of acetone, heat to 50°C and dissolve until clear to obtain a mixture;

[0036] 2) Slowly cool the mixture obtained in step 1) until the crystals are precipitated, then keep it warm at -5°C for 3 hours and stir to fully precipitate the crystals, filter, and use a mixed solvent at 0°C (this mixed solvent is the same as that used in step 1) Mixed solvent is the same), wash the solid, and dry at 50°C to obtain 94.55g of refined roxithromycin.

[0037] The mass yield of the purified roxithromycin obtained in the present embodiment is 94.55%.

Embodiment 2

[0039] The refining method of the roxithromycin of the present embodiment may further comprise the steps:

[0040] 1) Disperse 100g of crude roxithromycin in a mixed solvent formed by mixing 50ml of ethanol and 450ml of acetone, heat to 60°C and dissolve until clear to obtain a mixture;

[0041] 2) Slowly cool the mixture obtained in step 1) until the crystals are precipitated, then keep it warm at -20°C for 1.5 hours and stir to fully precipitate the crystals, filter, and use a mixed solvent at 5°C (this mixed solvent and step 1) The same mixed solvent used) washed the solid and dried at 55°C to obtain 85.78g of refined roxithromycin.

[0042] The mass yield of the purified roxithromycin obtained in the present embodiment is 85.78%.

Embodiment 3

[0044] The refining method of the roxithromycin of the present embodiment may further comprise the steps:

[0045] 1) Disperse 100g of crude roxithromycin in a mixed solvent formed by mixing 900ml of ethanol and 100ml of acetone, heat to 65°C and dissolve until clear to obtain a mixture;

[0046] 2) Slowly cool the mixture obtained in step 1) until the crystals are precipitated, then keep it warm at -10°C for 2 hours and stir to fully precipitate the crystals, then filter and use a mixed solvent at 5°C (this mixed solvent is the same as that used in step 1) Mixed solvent is the same), wash the solid, and dry at 65°C to obtain 88.74g of refined roxithromycin.

[0047] The mass yield of the purified roxithromycin obtained in the present embodiment is 88.74%.

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Abstract

The invention discloses a roxithromycin refining method comprising the following steps: (1) a roxithromycin crude product is dispersed in a mixed solvent formed by mixing lower alcohol and acetone; the mixture is heated until clarified, such that a mixture is obtained; (2) the mixture obtained in the step (1) is cooled until crystals are precipitated; the temperature is maintained at a low temperature and the material is stirred, or a polar solvent is dropped and the material is stirred, such that crystals are fully precipitated; and filtering, washing and drying are carried out, such that refined roxithromycin is obtained. According to the roxithromycin refining method, the mixed solvent formed by mixing lower alcohol and acetone is used for dispersing crude roxithromycin, and refining is carried out with heating dissolving and cooling precipitation processes, such that impurity removing effect is good, and product yield is high. The refined roxithromycin has high purity. The product has good color, uniform particle size, and low broken crystal amount. With the refining method, after fractionation recovery, the mixed solution can be reused. The amount of produced waste liquid is low, and cost is low. The process is simple, and operation is convenient. The method is suitable for large-scale industrial productions.

Description

technical field [0001] The invention belongs to the technical field of roxithromycin preparation, in particular to a method for refining roxithromycin. Background technique [0002] Roxithromycin is a new generation of macrolide antibiotics, a derivative of erythromycin, mainly acting on Gram-positive bacteria, anaerobic bacteria, chlamydia and mycoplasma. The antibacterial effect of roxithromycin in vitro is similar to that of erythromycin, and the antibacterial effect in vivo is 1-4 times stronger than that of erythromycin. It is clinically used for bronchitis, pneumonia, tonsillitis, ENT infection, and urinary system infection caused by sensitive bacteria. , skin and soft tissue infections. [0003] Roxithromycin molecular structure is: [0004] [0005] In the "European Pharmacopoeia 6.3" (EP6.3) version, the impurities involved in the roxithromycin part are A, B, C, D, E, F, G, H, I, J, K, and their specific sources are as follows : [0006] A——erythromycin A, br...

Claims

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Application Information

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IPC IPC(8): C07H17/08C07H1/06
Inventor 张听盼陈建晖李亚娥
Owner ZHENGZHOU HOUYI PHARMA
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