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Method for preparing Etimicin sulfate

A technology of etimicin sulfate and dilute sulfuric acid, applied in the field of medicine, can solve the problems of low total yield, low reaction selectivity, complicated separation procedures, etc., and achieves optimization of reaction conditions and separation conditions, shortening of synthesis process, synthesis of The effect of process shortening

Inactive Publication Date: 2011-11-23
JIANGXI JEMINCARE GRP CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The synthesis process of this patent has problems such as low reaction selectivity, complex synthesis route, complex separation procedure and low efficiency, large discharge of three wastes, and low overall yield.

Method used

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  • Method for preparing Etimicin sulfate
  • Method for preparing Etimicin sulfate
  • Method for preparing Etimicin sulfate

Examples

Experimental program
Comparison scheme
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Embodiment 1

[0045] Embodiment 1, preparation method of the present invention

[0046] Take 10kg of gentamicin C1a base, add 30kg of solvent DMSO, stir and dissolve, add cobalt sulfate to the solution, stir and cool down to 14°C at the same time. Ethyl p-toluenesulfonate was added to the obtained mixture, stirred and reacted at 12°C for 2.5 hours, the reaction solution was added with reagent sodium borohydride, reacted for 1.5 hours, and then the pH was adjusted to 12.0 with 3 mol / L ammonia water. The obtained reaction solution was adsorbed with macroporous resin, and washed with deionized water until there was no solvent smell. The washed macroporous resin was eluted with 20% ethanol, and the purity of etimicin in the eluate was detected by HPLC, and the eluate with a purity greater than 90% was collected. The obtained eluate was concentrated in vacuo to recover ethanol, and the recovered ethanol was adjusted to the previous step after adjusting its concentration. Add 15% activated carb...

Embodiment 2

[0047] Embodiment 2, preparation method of the present invention

[0048]Take 15kg of gentamicin C1a base, add 40kg of solvent methanol, stir and dissolve, add cobalt acetate to the solution, stir and cool down to 13°C at the same time. Diethyl carbonate was added to the obtained mixture, stirred and reacted at 13° C. for 2.8 hours, sodium borohydride was added to the reaction solution, reacted for 2 hours, and then the pH was adjusted to 12.5 with 4 mol / L ammonia water. The obtained reaction solution was adsorbed with macroporous resin, and washed with deionized water until there was no solvent smell. The washed macroporous resin was eluted with 25% ethanol, and the purity of etimicin in the eluate was detected by HPLC, and the eluate with a purity greater than 90% was collected. The obtained eluate was concentrated in vacuo to recover ethanol, and the recovered ethanol was adjusted to the previous step after adjusting its concentration. Add 18% activated carbon to the obta...

Embodiment 3

[0049] Embodiment 3, preparation method of the present invention

[0050] Take 12kg of gentamicin C1a base, add 50kg of solvent acetonitrile, stir and dissolve, add N-Boc to the solution, stir and cool down to 10°C at the same time. Add acetaldehyde to the obtained mixture, stir and react at 13.5° C. for 3 hours, add potassium borohydride to the reaction solution, react for 2.5 hours, and then adjust the pH to 13.5 with 4.5 mol / L ammonia water. The obtained reaction solution was adsorbed with macroporous resin, and washed with deionized water until there was no solvent smell. The washed macroporous resin was eluted with 18% ethanol, and the purity of etimicin in the eluate was detected by HPLC, and the eluate with a purity greater than 90% was collected. The obtained eluate was concentrated in vacuo to recover ethanol, and the recovered ethanol was adjusted to the previous step after adjusting its concentration. Add 10% activated carbon to the obtained concentrated solution,...

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Abstract

The invention relates to a method for preparing Etimicin sulfate. In the method, under the action of a complex protective agent, gentamicin Cla is subjected to 1-N-ethylation, the synthesized product is separated by macroporous resin, the synthesized product is concentrated, the pH value of the synthesized product is adjusted by sulfuric acid to form a salt, the salt is decolorized by active carbon and freeze-dried; and the medicinal Etimicin sulfate meeting related standards is obtained. When the method is used for producing Etimicin sulfate, the synthesis process can be shortened greatly, the labor production efficiency is improved, and the discharge of waste water, gas and slag is reduced.

Description

technical field [0001] The invention belongs to the field of medicine and relates to a preparation method of medicine, in particular to a new synthesis process of etimicin sulfate. 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] 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 effect on the following infections: Respiratory tract infections: such as acute bronchitis, acute exacerbation of chronic bro...

Claims

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Application Information

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IPC IPC(8): C07H15/236C07H1/00
Inventor 吴凌云
Owner JIANGXI JEMINCARE GRP CO LTD
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