Refinement method of erythromycin thiocyanate

A technology of erythromycin thiocyanate and a refining method, applied in the field of medicine, can solve problems such as low light transmittance of finished products, and achieve the effects of high light transmittance, low production and operation cost, and good product quality

Active Publication Date: 2016-05-25
四川新迪生物制药有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although the method provided by this patent application has improved the purity of erythromycin thiocyanate to a certain e

Method used

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  • Refinement method of erythromycin thiocyanate

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Embodiment 1

[0032] Embodiment 1 erythromycin thiocyanate refining method of the present invention

[0033] Get 400 grams of erythromycin thiocyanate crude product (moisture content 31.17%, erythromycin titer is 556u / mg; HPLC external standard method detects, contains erythromycin A73.37% in terms of dry product, contains erythromycin B3 .1%, containing erythromycin C1.72%, containing erythromycin E3.99%), adding methanol (adding 2.3 liters of methanol per billion units of erythromycin), stirring, using mixed alkali solution (sodium hydroxide and The molar ratio of sodium carbonate is 7:3, the concentration is 24%) to adjust the pH to 9.5, and the temperature is raised to 38±2°C, the insoluble matter is removed by centrifugation, and the filter cake is washed with methanol (washing with 0.2 liter of methanol per billion units of erythromycin) , combine the washing liquid and the centrifugation liquid, heat up to 41±2°C, add 40% sodium thiocyanate solution (0.4 mole sodium thiocyanate is ad...

Embodiment 2

[0037] Embodiment 2 erythromycin thiocyanate refining method of the present invention

[0038] Get 400 grams of erythromycin thiocyanate crude product (moisture content 31.17%, erythromycin titer is 556u / mg; HPLC external standard method detects, contains erythromycin A73.37% in terms of dry product, contains erythromycin B3 .1%, containing erythromycin C1.72%, containing erythromycin E3.99%), adding methanol (adding 2.3 liters of methanol per billion units of erythromycin), stirring, using mixed alkali solution (sodium hydroxide and The molar ratio of sodium carbonate is 7:3, the concentration is 20%) to adjust the pH to 9.4, and the temperature is raised to 38±2°C, the insoluble matter is removed by centrifugation, and the filter cake is washed with methanol (washing with 0.2 liter of methanol per billion units of erythromycin) , combine the washing liquid and the centrifugation liquid, heat up to 41±2°C, add 40% sodium thiocyanate solution (0.4 mole sodium thiocyanate is ad...

Embodiment 3

[0040] Embodiment 3 erythromycin thiocyanate refining method of the present invention

[0041]Get 400 grams of erythromycin thiocyanate crude product (water content 25.5%, erythromycin titer is 604u / mg; HPLC external standard method detects, contains erythromycin A77.72% in terms of dry product, contains erythromycin B2 .1%, containing erythromycin C2.9%, containing erythromycin E3.6%), add methanol (every billion units of erythromycin add 2.1 liters of methanol), stir, use mixed alkali solution (sodium hydroxide and The molar ratio of sodium carbonate is 6:4, the concentration is 20%) to adjust the pH to 9.5, and the temperature is raised to 38±2°C, the insoluble matter is removed by centrifugation, and the filter cake is washed with methanol (washing with 0.2 liter of methanol per billion units of erythromycin) , combine the washing liquid and the centrifugation liquid, heat up to 41±2°C, add 40% sodium thiocyanate solution (0.4 mole sodium thiocyanate is added for every mol...

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Abstract

The invention provides a refinement method of thiocyanate erythromycin. The method comprises the following steps: a. taking an erythromycin thiocyanate crude product, adding a solvent and a mixed alkali solution for dissolution, and removing insoluble substances to obtain a supernatant, wherein the mixed alkali solution is a water solution comprising sodium hydroxide and sodium carbonate, the mole ratio of the sodium hydroxide to the sodium carbonate in the mixed alkali solution is 9:1-1:9, and the solvent is an alcohol solvent or acetone; and b. adding sodium thiocyanate into the supernatant in the step a, regulating the pH value to 6.0-9.0, crystallizing, filtering, and drying to obtain the erythromycin thiocyanate finished product. The erythromycin thiocyanate finished product prepared by the method has the advantages of high light transmittance, high yield and high product quality, and has favorable industrial application prospects.

Description

technical field [0001] The invention belongs to the field of medicine, in particular to a method for refining erythromycin thiocyanate. Background technique [0002] Erythromycin Thiocyanate (Erythromycin Thiocyanate, referred to as sulfur red) is the thiocyanate of erythromycin, which is a white or off-white crystalline powder. It is a macrolide antibiotic for animals. At the same time, thiocyanate Erythromycin acid can also be used to synthesize clarithromycin, roxithromycin and azithromycin and other semi-synthetic erythromycins that are popular at home and abroad, and it is an important pharmaceutical intermediate. Therefore erythromycin thiocyanate is as drug raw material, and its quality just seems particularly crucial. [0003] An important control factor of drug quality is the content of impurities. The less impurities the drug contains, the lower the incidence of clinical adverse reactions and the better the safety. The same is true for the preparation of medicine...

Claims

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Application Information

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IPC IPC(8): C07H17/08C07H1/06
CPCC07H1/06C07H17/08
Inventor 常翔宇赵鑫努尔买买提·库达巴尔地张翔程伶俐张亚勇臧静沙泥燕木·努尔买买提
Owner 四川新迪生物制药有限公司
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