Method for purifying roxithromycin

A roxithromycin, a certain amount of technology, applied in the field of purification technology of roxithromycin, can solve the problems such as the decline of the effect and the difficulty in meeting the production needs, and achieve the effect of good effect, low cost and less three wastes

Inactive Publication Date: 2011-10-19
ZHEJIANG GUOBANG PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Integrating the method of this document, considering the environmental protection of solvent, cost and the drug effect of different crystal forms of roxithromycin, it is better to use ethanol / water, acetone / water, through the comparative test with the document method, it is found that if roxithromycin If other impurities in the crude product, such as impurity F, impurity G, and impurity K, etc. are also large, the effect of these two systems will drop a lot, and it is difficult to meet the production needs

Method used

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  • Method for purifying roxithromycin

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Experimental program
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Effect test

Embodiment 1

[0041] Add 15ml of methanol and 15ml of ethanol to 30g of crude roxithromycin as a mixed solvent, mix the three and raise the temperature to 50°C~65°C to dissolve and clarify, then cool slowly, and keep stirring at -5°C after the crystals are precipitated After 3 hours, filter, wash the solid with a small amount of the above mixed solvent at 0-5°C, and dry at 50-55°C to obtain 28.7g of roxithromycin.

[0042] After testing, the HPLC content was 98.26%, impurity A was not detected, impurity B was 0.05%, impurity C was 0.07%, impurity D was 0.03%, impurity E was 0.06%, impurity F was 0.31%, impurity G was 0.04%, impurity H 0.21%, impurity I 0.21%, impurity J 0.15%, impurity K 0.12%. The mass yield is 95.67%.

Embodiment 2

[0044] Add a mixed solution consisting of 150ml methanol and 150ml ethanol to 30g roxithromycin crude product, mix the three to form a mixed system, and raise the temperature to 50°C~65°C to dissolve and clarify, then cool slowly, and wait for the crystals to separate out at -5 Continue to heat and stir for 3 hours at ℃, filter, wash the solid with a small amount of mixed solvent at 0-5 ℃, and dry at 50-55 ℃ to obtain 13.2 g of roxithromycin.

[0045] After testing, the HPLC content was 99.44%, impurity A was not detected, impurity B was 0.03%, impurity C was 0.05%, impurity D was not detected, impurity E was 0.04%, impurity F was 0.05%, impurity G was not detected, Impurity H 0.08%, impurity I 0.08%, impurity J 0.05%, impurity K 0.07%. The mass yield is 44%.

Embodiment 3

[0047] Add a mixed solution consisting of 90ml methanol and 90ml ethanol to 30g crude roxithromycin, mix the three to form a mixed system, and raise the temperature to 50°C~65°C to dissolve and clarify, then cool slowly, and wait for crystals to separate out at -5 Continue to heat and stir for 3 hours at ℃, filter, wash the solid with a small amount of mixed solvent at 0-5 ℃, and dry at 50-55 ℃ to obtain 21.3 g of roxithromycin.

[0048] After testing, the HPLC content was 98.90%, impurity A was not detected, impurity B was 0.05%, impurity C was 0.05%, impurity D was 0.03%, impurity E was 0.02%, impurity F was 0.15%, impurity G was not detected, Impurity H 0.19%, impurity I 0.15%, impurity J 0.11%, impurity K 0.11%. The mass yield is 71%.

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Abstract

The invention mainly discloses a method for purifying roxithromycin. The method comprises the following steps of dispersing erythromycin crude products into a mixed solvent of two lower alcohols, heating to clarify the mixed liquid obtained from the above step, cooling to make precipitates be separated from the clarified liquid obtained from the above step and stirring at a low temperature for a period of time to make the precipitates be separated from the clarified liquid fully, and filtering to obtain purified erythromycin. The method has the advantages of good impurity removal effects, high yield, continuous use feature of mother liquor, few three wastes, low cost, good adaptability for industrialization production, and favorable products with uniform granularity, good fluidity, a small number of broken crystals, and high hardness of crystals.

Description

technical field [0001] The invention relates to the technical field of roxithromycin, in particular to a purification process of roxithromycin. Background technique [0002] The molecular structure of roxithromycin is shown in (I) below, [0003] [0004] 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, among which the impurities [0005] A——erythromycin A, brought from raw materials [0006] B—Destruction product of declardinose [0007] C——erythromycin A oxime, brought in raw materials [0008] D——trans-roxithromycin, generated from trans-oxime [0009] E—Roxithromycin C, produced from erythromycin C oxime [0010] F——N-demethylroxithromycin, generated from N-demethyloxime [0011] G——The impurities in the side chain react with oxime [0012] H—Roxithromycin B, produced from erythromycin B oxime [0013] I - double substituted roxithromycin [0014] J——The impurities in t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H17/08C07H1/06
Inventor 邱家军苗正发田利焕金勇王兆刚王凤江候仲轲叶九胜
Owner ZHEJIANG GUOBANG PHARMA
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