Etimicin sulfate preparation method

A technology of etimicin sulfate and reaction solution, which is applied in the preparation of sugar derivatives, chemical instruments and methods, sugar derivatives, etc., can solve the problems of many side reactions, low yield, and a large amount of waste liquid, and achieve simple operation , Ease of industrialization, and the effect of reducing the amount of waste liquid

Active Publication Date: 2016-04-27
WUXI JIMIN KEXIN SHANHE PHARMA +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This process has problems such as lengthy synthesis route and low yield; two macroporous resin purifications, resulting in a large amount of waste liquid; no functional group protection step when adding acetaldehyde, and many side reactions.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Get gentamicin C1a base, add methanol with 6 times the weight of gentamicin C1a base, stir and dissolve to obtain a solution, add 2 times the equivalent of cobalt acetate of the amount of gentamicin C1a base, stir to obtain reaction solution 1, Add p-methoxybenzaldehyde equivalent to 4 times the amount of gentamicin C1a base substance, stir and react for 2 hours to obtain reaction solution 2, add ammonium oxalate 2 times the amount of gentamicin C1a base substance, filter after stirring , to get reaction solution 3, add acetyl chloride of 2 times the equivalent of the amount of gentamicin C1a base substance, stir and react for 2 hours, get reaction solution 4, add 7 times the equivalent of gentamicin C1a base substance amount of hydroboration Potassium, stirred and reacted for 6 hours to obtain the reaction solution 5, adding 5 times the volume of water, vacuum concentration to remove the solvent under the condition that the vacuum degree is not higher than 0.2 atmospher...

Embodiment 2

[0021] Get gentamicin C1a base, add 7 times of dichloromethane of gentamicin C1a base weight, stir and dissolve to obtain a solution, add 3 times the equivalent of gentamicin C1a base material, and stir to obtain reaction solution 1 , add the trityl chloride of 6 times equivalent of the amount of gentamicin C1a base material, stir and react for 3 hours, get reaction solution 2, add the ammonium phosphate of 2-4 times of the amount of gentamicin C1a base material, stir After filtration, get reaction solution 3, add the glacial acetic acid of 3 times equivalents of the amount of gentamicin C1a base substance, stir and react for 3 hours, get reaction solution 4, add 10 times equivalents of the amount of gentamicin C1a base substance Sodium triacetoxyborohydride was stirred and reacted for 4 hours to obtain a reaction solution 5, which was added to 5 times the volume of water and concentrated in vacuo under the condition that the vacuum degree was not higher than 0.2 atmospheric pr...

Embodiment 3

[0023] Get gentamicin C1a base, add DMSO 10 times the weight of gentamicin C1a base, stir and dissolve to obtain a solution, add 2-3 times the amount of gentamicin C1a base zinc sulfate, stir to obtain reaction solution 1, Add dimethoxybenzaldehyde with 3 times the amount of gentamicin C1a base substance, stir and react for 1 hour to obtain reaction solution 2, add potassium phosphate with 2-4 times the amount of gentamicin C1a base substance, and stir Filter to obtain reaction solution 3, add acetic anhydride with 1.5 times the amount of gentamicin C1a base substance, stir and react for 1 hour to obtain reaction solution 4, add cyanoborohydrogenation with 5 times the amount of gentamicin C1a base substance Sodium, stirred and reacted for 4 hours to obtain reaction solution 5, added 3 times the volume of water, concentrated in vacuum to remove the solvent under the condition that the vacuum degree below 80°C was not higher than 0.2 atmospheres, adjusted the pH to 13 with ammoni...

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PUM

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Abstract

The invention provides an etimicin sulfate preparation method. The method comprises the following steps: taking gentamycin C1a base, dissolving the gentamycin C1a base in a certain proportion of a solvent, adding a certain proportion of a complexing agent to complex, adding a certain proportion of an amino group protection agent, keeping for a certain time, adding a certain proportion of a precipitating agent, stirring above materials, filtering the obtained mixture, adding a certain proportion of an acetylation reagent to the above obtained filtrate, reacting for a certain time, adding a certain proportion of a reducing agent, reacting for a certain time, removing an amino protection group, adding a certain proportion of water, carring out vacuum concentration under certain conditions to remove the solvent, adjusting the pH value with ammonia water, adsorbing with macro-porous resin, carrying out gradient separating purification with diluted ethanol, collecting an etimicin solution with a certain purity, carrying out vacuum concentration under certain conditions, adding sulfuric acid to adjust the pH value, adding a certain proportion of active carbon, decolorizing, filtering, and drying to obtain etimicin sulfate according with relevant standards.

Description

Technical field: [0001] The invention relates to the field of medicinal chemistry, and relates to a preparation method of aminoglycoside compounds, in particular to a preparation method of etimicin sulfate. Background technique: [0002] Etimicinsulfate (Etimicinsulfate) is a new generation of semi-synthetic aminoglycoside antibiotics with high efficiency, low toxicity and resistance to drug-resistant bacteria with independent intellectual property rights. It is the only antibiotic that has obtained the national first-class new drug certificate. Infectious medicines. [0003] Etimicin sulfate injection is suitable for Escherichia coli, Klebsiella pneumoniae, Serratia spp., Citrobacter spp., Enterobacter spp., Acinetobacter spp., Proteus spp. Bacteria, Pseudomonas aeruginosa and Staphylococcus caused by various infections. Clinical studies have shown that this product has a good curative effect on the following infections. Respiratory tract infection: such as acute bronchi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H15/236C07H1/00
CPCC07H1/00C07H15/236
Inventor 吴凌云姜迎庆墙广灿薛超一易斌
Owner WUXI JIMIN KEXIN SHANHE PHARMA
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