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Dynamic controlled crystalline method of preparing erythromycin from erythromysin salt

A dynamic control and erythromycin technology, applied in sugar derivatives, organic chemistry, etc., can solve the problems of unstable quality of erythromycin, low qualified rate of primary crystallization potency, etc., and achieve the effect of stable product quality

Inactive Publication Date: 2004-07-21
EAST CHINA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, judging from the existing production implementation, both the "one-step method" and the "two-step method" have the problem that the quality of erythromycin is unstable, that is, the qualified rate of the primary crystallization potency of the product is low.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Put 65kg of erythromycin lactate into the alkali-transforming kettle, add 325L of acetone, stir and heat up to 25°C, add ammonia water, adjust the pH to 9.95, and remove the lower aqueous phase after standing still; 1.5KW / M 3 Stir and heat up to 50°C under certain conditions, and use continuous flow of water to dissolve and crystallize. The amount of water added is 420L. During this period, the stirring power range is adjusted in stages according to the crystallization status. The range is 0.1KW / M 3 ~0.6KW / M 3 Between, the time is 8h; then enter the crystal growth stage, control the stirring power to 0.6KW / M 3 , the time is 18h, the crystallization process is over, at this time the temperature of the whole system drops to 20°C; filter, wash the wet crystals with 550L of 50°C water; dry to obtain 41.42kg of erythromycin base product, the wet base potency is 887.0u / mg , moisture 4.9%, dry basis potency 932.7u / mg, once-transbasic crystallization weight yield 63.7%, poten...

Embodiment 2

[0019] Put 180kg of erythromycin lactate into the alkali-transforming kettle, add 940L of acetone, stir and heat up to 28°C, add ammonia water, adjust the pH to 9.95, and remove the lower water phase after standing still; 2.5KW / M 3 Stir and heat up to 38°C under certain conditions, and dissolve and crystallize by adding water continuously. The amount of water added is 1860L. During this period, the stirring power range is adjusted in stages according to the crystallization status to 0.1KW / M 3 ~0.6KW / M 3 Between, the time is 3h; then enter the crystal growth stage, control the stirring power to 0.5KW / M 3 , the time is 25h, the crystallization process is over, at this time the temperature of the whole system drops to 30°C; filter, wash the wet crystals with 1850L of 50°C water; dry to obtain 108.0kg of erythromycin base product, its dry basis potency is 925u / mg, The water content is 4.8%, the crystallization weight yield of one-time alkali conversion is 60.0%, and the potency ...

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Abstract

A process for preparing erythromycin from erythromycin salt by dynamically controlled coystallizing method in which the temp and stirring intensity are varied includes beginning crystallizing at high temp under strong stirring, educing crystal by varying stirring intensity and nursing crystal by varying stirring intensity and continuously cooling. Its advantage is high purity.

Description

technical field [0001] The invention relates to a preparation method of erythromycin, in particular to a method for preparing erythromycin from erythromycin salt through alkali conversion and crystallization. Background technique [0002] Erythromycin is a widely used macrolide antibiotic. In addition to being directly used as a medicine, it is also used as a raw material for the production of various semi-synthetic erythromycin products. Erythromycin is produced by fermentation and is a weakly alkaline product that is insoluble in water but easily soluble in organic solvents such as butyl acetate, ethanol, acetone, and chloroform. [0003] For the method of extracting erythromycin from the erythromycin fermentation broth, various separation processes such as extraction and adsorption can be used, and the subsequent refining of the product can adopt the method of low-temperature crystallization or chemical methods. At present, an extraction process commonly used by erythrom...

Claims

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Application Information

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IPC IPC(8): C07H17/08
Inventor 陈葵朱家文武斌纪利俊郭建国
Owner EAST CHINA UNIV OF SCI & TECH
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