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Synthesis method of etimicin sulfate intermediate (3,2',6'-tri-N-acetyl gentamicin C1a)

A technology of etimicin sulfate and gentamycin, applied in chemical instruments and methods, preparation of sugar derivatives, sugar derivatives, etc., can solve the problems of etimicin sulfate with many impurities and difficult purification, and achieve The effect of reducing the use of solvents, reducing energy consumption, and reducing emissions

Active Publication Date: 2014-01-22
WUXI JIMIN KEXIN SHANHE PHARMA +1
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AI Technical Summary

Problems solved by technology

[0012] In the above-mentioned patents, the purity of the finished product of 3,2',6'-tri-N-acetylgentamycin C1a is only 92%, which brings more impurities to the further preparation of etimicin sulfate and makes purification difficult

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] a. Add 20L of methanol and 2.70kg of gentamicin C to a 50L three-necked flask at a temperature of 20°C 1a And the anhydrous zinc acetate of 3.21kg, stir 1.5 hours to dissolve, get gentamicin C 1a -Zn complexes.

[0022] b. Add dropwise 2.55 L of acetic anhydride to step a for acetylation.

[0023] c. After the reaction is completed, the reaction solution in step b is concentrated, and the concentrated solution is passed into a chromatographic separation column for sample loading, rinsed without salt water, analyzed with ethanol aqueous solution, and the effective components are collected. Concentrate and dry to obtain 3.29kg of P1 finished product. The yield was 95.3%, and the purity was 96.1%.

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Abstract

The invention relates to a synthesis method of an etimicin sulfate intermediate (3,2',6'-tri-N-acetyl gentamicin C1a). The synthesis method comprises the following steps: a, adding 20 L of methanol, 2.70 kg of gentamicin C1a and 3.21 kg of anhydrous zinc acetate into a 50 L three-port bottle at a temperature of 29 DEG C, stirring for 1.5 h to dissolve, and thus obtaining a gentamicin C1a-Zn complex; b, dripping 2.55 L of acetic anhydride into the complex of the step a for acetylation; c, after finishing the reaction, concentrating the reaction liquid of the step b, introducing the concentrated liquid into a chromatographic separation column for charging the sample, rinsing with a salt-free water, resolving with an ethanol water solution, and collecting effective components; concentrating, drying to obtain 3.29 kg of the finished product P1, wherein the yield is 95.3%, and the purity is 96.1%.

Description

technical field [0001] The invention relates to the field of medicinal chemistry, in particular to a method for synthesizing aminoglycoside antibiotic drug intermediate 3,2',6'-tri-N-acetyl gentamycin C1a. Background technique [0002] Etimicin sulfate (Etimicin sulfate) is a new generation of semi-synthetic aminoglycoside antibiotics with independent intellectual property rights, which is highly efficient, low-toxic, and resistant to drug-resistant bacteria. It is the only one that has obtained the national first-class new drug certificate. Anti-infective drugs. [0003] At present, for the intermediate 3,2',6'-tri-N-acetylgentamycin C1a (abbreviation: P1), Chinese patent documents have successively disclosed three preparation methods. [0004] Chinese patent 93112412.3 describes the following method: [0005] At room temperature, 10 g of GMC1a freeze-dried powder was dissolved in 40 ml of water under stirring, 360 ml of dimethylformamide was added, and 20 g of CoAc2·4H2O...

Claims

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Application Information

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IPC IPC(8): C07H15/236C07H1/00
Inventor 姜迎庆吴凌云郭永忠邹济高杨春艳
Owner WUXI JIMIN KEXIN SHANHE PHARMA
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