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Preparation method of low content 25-deacetyl rifamycin S

A technology for deacetylation and rifamycin, applied in the field of preparation of rifamycin S acid, achieves high yield, strong controllability, and reduced production cost

Inactive Publication Date: 2014-03-19
LUOHE NANJIECUN PHARMA GRP PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, according to the novelty of science and technology, there is no method for preparing rifamycin S acid by double-solvent extraction, feeding acidification and recrystallization technology, and obtaining the low 25-position deacetylation component S acid, high purity, and high yield product. Related literature and published patent reports

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] ⑴ Dissolution Put ethanol and water into a stirring tank, heat up to 30°C and put in S-Na salt, the mass ratio of ethanol: water: S-Na salt is 5:1:3, and then add 9 mol / L sulfuric acid solution , the acid addition rate is 0.02 L / Lmin, the time is within 70 minutes, the process temperature is controlled below 50°C, and the stirring speed is 30 rpm at the same time, and then the temperature is lowered to below 5°C, static, and filtered;

[0027] ⑵ Beating Add the wet crude product after rejection filtration to the solvent ethanol in a ratio of 1:1 to prepare a slurry, and stir and beat for 60 minutes at a temperature of 4°C, then shake and filter;

[0028] (3) Washing: Add pure water of 10 times the quality of the wet product obtained after beating and filtering to the washing tank, adjust the pH to 3 with sulfuric acid, then add the wet product obtained after beating and filtering, stir for 30 minutes and then filter;

[0029] (4) Recrystallization Add isopropanol 10 tim...

Embodiment 2

[0032] ⑴ Dissolution Put ethanol and water into a stirring tank, heat up to 40°C and put in S-Na salt, the mass ratio of ethanol: water: S-Na salt is 5:1:3, and add 9 mol / L sulfuric acid solution , the acid addition rate is 0.03 L / Lmin, the time is within 60 minutes, the process temperature is controlled below 50°C, and the stirring speed is 30 rpm at the same time, and then the temperature is lowered to below 5°C, static, and filtered;

[0033] ⑵ Beating Add the wet crude product after rejection filter to solvent ethanol in a ratio of 1:2 to prepare a slurry, stir and beat for 80 minutes at a temperature of 4°C, and then shake filter;

[0034] (3) Water washing: Add pure water of 10 times the quality of the wet product obtained after beating and filtering to the washing tank, adjust the pH to 4.5 with sulfuric acid, then add S acid after beating, stir for 60 minutes and then filter;

[0035] (4) Recrystallization Add isopropanol 10 times the mass of the material after washing...

Embodiment 3

[0038] ⑴ Dissolution Put ethanol and water into a stirring tank, heat up to 35°C and put in S-Na salt, the mass ratio of ethanol: water: S-Na salt is 5:1:3, and add 9 mol / L sulfuric acid solution , the acid addition rate is 0.025 L / Lmin, the time is within 65 minutes, the process temperature is controlled below 50°C, and the stirring speed is 30 rpm at the same time, and then the temperature is lowered to below 5°C, static, and filtered;

[0039] ⑵ Beating Add the wet crude product after rejection filter to solvent ethanol in the ratio of 2:3 to prepare a slurry, and stir and beat for 70 minutes at a temperature of 4°C, and then shake filter;

[0040] (3) Water washing: Add pure water of 10 times the quality of the wet product obtained after beating and filtering to the washing tank, adjust the pH to 3.5 with sulfuric acid, then add S acid after beating, stir for 40 minutes and then filter;

[0041] (4) Recrystallization Add isopropanol 10 times the mass of the material washed...

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PUM

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Abstract

The invention discloses a preparation method of low content 25-deacetyl rifamycin S. In a preparation process, the rifamycin S which is low in deacetylation S acid impurity (less than 1.0%), high in purity (higher than 97%), in the form of orange-yellow crystalline powder, and satisfies quality requirements of manufacturers at home and abroad is prepared by controlling key technical parameters such as feeding velocity of sulfuric acid, a rate of charge of materials to double solvents (alcohol and isopropanol), a pH value in a water-washing process and a cooling rate in a recrystallization process. The novel method has the advantages of being clear in control index, easy to operate, strong in controllability, high in yield and stable in product quality, and can be applied to mass preparation of the rifamycin S acid in a fermentation production process.

Description

technical field [0001] The invention relates to a preparation method of rifamycin S acid, which is a deacetylated component at the 25th position, and belongs to the downstream technical field of separation and purification of secondary metabolites. Background technique [0002] Rifamycin is the general term for semi-finished antibiotics such as rifampin and rifampin, which have strong antibacterial or antibacterial effects on Mycobacterium tuberculosis and other mycobacteria (including Bacillus leprae, etc.). High-quality rifamycin S-Na salt and S acid are the important basis for the final synthesis of high-quality rifamycin series drugs, especially the main impurity of rifamycin S acid---25-position deacetylation component S The control requirements of the acid content in the international market are more stringent. [0003] At present, the separation and purification process of rifamycin S acid at home and abroad mostly adopts the solvent extraction process under acidic c...

Claims

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Application Information

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IPC IPC(8): C07D498/08
CPCC07D498/08
Inventor 李盘欣孔爱卿张立翔王志黄亚男
Owner LUOHE NANJIECUN PHARMA GRP PHARMA
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