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Synthesis process of erythromycin oxime

A technology of erythromycin oxime and a synthesis method, which is applied in the synthesis field of erythromycin oxime, can solve the problems of high temperature and pH control requirements, complicated processes and the like, and achieves the effects of simple operation, safe and reliable operation

Inactive Publication Date: 2005-09-28
镇江新宇化工有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These methods are complex in the process of synthesis reaction, and have high requirements on the control of temperature and pH

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0008] Heat 100L of erythromycin fermented pre-extracted solution, that is, mixed butyl acetate extract, to 30°C in a reaction kettle, add 2% of the total volume of saturated saline, stir for 0.5-1 hour, and let it stand for more than 2 hours , to remove the lower layer of water and impurities. The mixed butyl acetate extract of the above-mentioned purified erythromycin is warmed up to 40°C, and is added in a stirring state by the weight ratio of hydroxylamine hydrochloride: triethylamine=1.5:1. The purpose of this operation is to control the reaction solution at pH = 5.5, stir at 30°C for 16-24 hours, monitor the reaction with a common thin-layer chromatography method, separate the reaction liquid from solid to liquid, and the solid is erythromycin oxime hydrochloride. Then the solid erythromycin oxime hydrochloride of gained is dropped in the reaction kettle by the weight ratio of solid erythromycin oxime hydrochloride: methyl alcohol=1: 1.5, keep temperature 10 ℃, adjust so...

Embodiment 2

[0010] Heat 100L erythromycin fermented pre-extracted liquid, that is, mixed butyl acetate extract, to 40°C in a reaction kettle, add saturated saline water accounting for 4% of the total volume, stir for 0.5-1 hour, and let it stand for more than 2 hours , to remove the lower layer of water and impurities. The mixed butyl acetate extract of the above-mentioned purified erythromycin is warmed up to 55°C, and is added in a stirring state by the weight ratio of hydroxylamine hydrochloride: triethylamine=2:1. The purpose of this operation is to control the reaction solution at pH = 6, stirred at 60°C for 16-24 hours, and after the reaction was monitored by common thin-layer chromatography, the reaction liquid was separated from solid to liquid, and the solid was erythromycin oxime hydrochloride. Then the solid erythromycin oxime hydrochloride of gained is dropped in the reaction kettle by the weight ratio of solid erythromycin oxime hydrochloride: methyl alcohol=1: 2, keep temper...

Embodiment 3

[0012] Heat 100L erythromycin fermented pre-extracted liquid, that is, mixed butyl acetate extract, to 50°C in a reaction kettle, add 5% of the total volume of saturated saline, stir for 0.5-1 hour, and let it stand for more than 2 hours , to remove the lower layer of water and impurities. The mixed butyl acetate extract of the above-mentioned purified erythromycin is warmed up to 70°C, and is added in a stirring state by the weight ratio of hydroxylamine hydrochloride: triethylamine=2.5:1. The purpose of this operation is to control the reaction solution at pH = 7, stirred at 70°C for 16-24 hours, and after the reaction was monitored by common thin-layer chromatography, the reaction liquid was separated from solid to liquid, and the solid was erythromycin oxime hydrochloride. Then the solid erythromycin oxime hydrochloride of gained is dropped in the reaction kettle by the weight ratio of solid erythromycin oxime hydrochloride: methyl alcohol=1:3, keep temperature 30 ℃, adjus...

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Abstract

The present invention discloses the synthesis process of 9-erythromycin oxime. Erythromycin oxime is synthesized through compounding hydroxylamine hydrochloride and triethylamine, and the direct synthesis of 9-erythromycin oxime with erythromycin fermenting extract liquid through the steps of synthesizing erythromycin oxime hydrochloride, creating methanol solution of erythromycin oxime and creating crystal liquid. The said process is simple, safe and reliable, and has product yield up to 70 % and purity over 93 %.

Description

Technical field [0001] The invention relates to a synthesis method of erythromycin oxime. Background technique [0002] 9-erythromycin oxime, referred to as erythromycin A oxime for short, is an intermediate for the synthesis of macrolide broad-spectrum antibiotics erythromycin and other drugs. The yield and purity of 9-erythromycin oxime directly affect the erythromycin The effect of the drug. In the current synthetic methods of erythromycin A oxime, some synthetic raw materials are easy to obtain but the yield is low; although some synthetic methods have high yield, they have high requirements on process conditions, the raw materials are easy to decompose, and the safety is poor. At present, the more common synthesis method is to condense erythromycin A and hydroxylamine hydrochloride to generate erythromycin oxime in an acid-base buffer solution, or to convert erythromycin oxime into erythromycin oxime by using hydroxylamine hydrochloride triethylamine acetic acid system...

Claims

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Application Information

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IPC IPC(8): C07H17/08
Inventor 林广德丁德平
Owner 镇江新宇化工有限责任公司
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