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Preparation method of erythromycin thiocyanate

A technology of erythromycin thiocyanate and sodium thiocyanate, which is applied in the preparation of sugar derivatives, chemical instruments and methods, sugar derivatives, etc., can solve problems such as high pollution, improve product purity, reduce sewage discharge, The effect of reducing the volume of sewage

Active Publication Date: 2019-07-12
HEC PHARM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of this invention is to provide a kind of preparation method of erythromycin thiocyanate, in order to solve the defect that more pollution is caused in purifying erythromycin thiocyanate in the prior art, prepare high-purity erythromycin thiocyanate, Finally, reduce the discharge of sewage under the premise of ensuring its stable quality

Method used

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  • Preparation method of erythromycin thiocyanate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] A preparation method of erythromycin thiocyanate, said method comprising the following steps:

[0030] Step 1, get a portion of crude product erythromycin thiocyanate, measure component content, chemical potency, moisture and weight, and calculate the titer billion (u) of this batch of materials.

[0031] Step 2. Add acetone to the reaction kettle, start stirring, and then heat up. When the temperature of the acetone rises to 40° C., put the crude product erythromycin thiocyanate in step 1, and start to slowly add the sodium hydroxide solution dropwise at the same time. The pH value of the final control system is 9.0, and the material temperature is 45°C.

[0032] Step 3, primary phase separation: After the crude product erythromycin thiocyanate dissolves completely, add required sodium chloride (the weight of sodium chloride: crude product erythromycin thiocyanate weight × crude product red thiocyanate) to the system once Loss on drying of mycin × 10%). After adding ...

Embodiment 2

[0041] A preparation method of erythromycin thiocyanate, said method comprising the following steps:

[0042] Step 1, get a batch of crude product erythromycin thiocyanate, measure component content, chemical potency, moisture and weight, and calculate the titer billion (u) of this batch of material.

[0043] Step 2, add acetone to the dissolving tank, start stirring, then heat up, when the temperature of acetone rises to 40°C, put the crude product erythromycin thiocyanate in step 1, and start to drop 30% sodium hydroxide solution at the same time , the pH value of the final system is 9.5, and the material temperature is 45°C.

[0044] Step 3, primary phase separation: After the crude product erythromycin thiocyanate dissolves completely, add required sodium chloride (the weight of sodium chloride: crude product erythromycin thiocyanate weight × crude product red thiocyanate) to the system once Loss on drying of mycin × 10%). Stir at 85 rpm for 5 min after adding sodium chl...

Embodiment 3

[0054] A preparation method of erythromycin thiocyanate, said method comprising the following steps:

[0055] Step 1, get a batch of crude product erythromycin thiocyanate, measure component content, chemical potency, moisture and weight, and calculate the titer billion (u) of this batch of material.

[0056] Step 2. Add a mixture of acetone and dichloromethane (volume ratio = 1:2.0-3.5) into the dissolution tank, start stirring, and then heat up. When the temperature of the mixed solvent rises to 30°C, the crude sulfur in step 1 Erythromycin cyanate was added, and 30% sodium hydroxide solution was added dropwise at the same time, the final system pH was 9.4, and the material temperature was 30°C.

[0057] Step 3, primary phase separation: After the crude product erythromycin thiocyanate dissolves completely, add required sodium chloride (the weight of sodium chloride: crude product erythromycin thiocyanate weight × crude product red thiocyanate) to the system once Loss on dr...

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Abstract

The invention relates to the technical field of crystallization engineering, in particular to a preparation method of erythromycin thiocyanate. The method comprises the following steps that a solventis added into crude erythromycin thiocyanate, a sodium hydroxide solution is used for regulating the pH value, and a mixed solution is obtained; sodium chloride solids are added into the mixed solution, standing is performed after stirring is performed, and phase splitting is performed to a supernate I; then, a saturated sodium chloride solution continues to be added into the supernate I, standingis performed after stirring is performed, phase splitting is performed, and a supernate II is obtained; a sodium thiocyanate solution is added into the supernate II, then, glacial acetic acid is added to regulate pH, reduced pressure distillation is performed, cooling is performed to reach 15-30 DEG C, and centrifuging is performed to obtain a wet erythromycin thiocyanate product; the wet erythromycin thiocyanate product is smashed and dried to obtain erythromycin thiocyanate. The preparation method of the erythromycin thiocyanate has the advantages that the technology is simple, control is easy, little wastewater is produced, the yield of the prepared erythromycin thiocyanate is high, and the purity of the prepared erythromycin thiocyanate is high.

Description

technical field [0001] The invention relates to the field of biopharmaceuticals, in particular to a preparation method of erythromycin thiocyanate. Background technique [0002] Erythromycin Thiocyanate (Erythromycin Thiocyanate) is an intermediate of the macrolide antibiotic erythromycin. Erythromycin is an antibiotic isolated from the culture solution of Saccharopolyspora rubrum in 1952. Erythromycin A, B, C, D, E and other components are separated from the solution, among which erythromycin A is the main component, which has strong antibacterial activity and less toxic and side effects; other components have weak antibacterial activity and are less toxic. The side effects are bigger than A. Commonly referred to as erythromycin thiocyanate refers to erythromycin A and its salts. This product is generally used as a pharmaceutical intermediate as a starting material for the subsequent synthesis of erythromycin derivatives. [0003] At present, erythromycin thiocyanate is ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H17/08C07H1/06
CPCC07H1/06C07H17/08
Inventor 李峰商清海周扬
Owner HEC PHARM CO LTD
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