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Refining method of isepamicin

A technology of isopamicin and refining method, which is applied in the field of biomedicine, can solve the problems of poor product quality stability and long cycle, and achieve the effect of good product stability and simplified purification process

Inactive Publication Date: 2019-02-15
ZHUOHE PHARM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The purpose of the present invention is to disclose a method for refining isopamicin, which does not use ion-exchange column chromatography purification, and overcomes the problems of long cycle and poor product quality stability caused by ion-exchange column chromatography purification in the prior art , the present invention can purify the crude product of isopamicin by a simple chemical method, simplifies the purification process of isopamicin, has good product stability, and is suitable for industrial mass production

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  • Refining method of isepamicin

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Effect test

Embodiment 1

[0027] The present embodiment carries out the refinement of isopamicin according to the method described above, and the specific steps are as follows:

[0028] Add 200ml of dichloromethane, 10g of crude isopamicin, 5.2g of anhydrous potassium carbonate and 2ml of benzyl bromide into a 1L reaction flask in sequence, stir magnetically, heat and reflux for 5 hours, judge the end of the reaction by TLC, filter with suction, and wash the filtrate with water until neutral , dried overnight over anhydrous sodium sulfate, and concentrated to obtain 13.8 g of isopamicin benzyl ether.

[0029] Add 10 g of isopamicin benzyl ether to a 250 ml round-bottom flask, add 105 ml of isopropanol / water (5 / 2), heat to reflux for 1 hour, and heat suction filtration. After the filtrate naturally cools to room temperature, stir overnight at 0°C for crystallization, and suction filtration. The filter cake was washed with a small amount of ethanol to obtain 8.2 g of white crystals, namely isopamicin ben...

Embodiment 2

[0033] The present embodiment carries out the refinement of isopamicin according to the method described above, and the specific steps are as follows:

[0034] Add 200ml of dichloromethane, 10g of crude isopamicin, 3.5ml of triethylamine and 2ml of benzyl bromide into a 1L reaction flask in sequence, stir magnetically, heat and reflux for 5 hours, judge the end of the reaction by TLC, filter with suction, wash the filtrate with water until neutral, Dry over anhydrous sodium sulfate overnight, and concentrate to obtain 14.0 g of isopamicin benzyl ether.

[0035] Add 10 g of isopamicin benzyl ether to a 250 ml round bottom flask, add 105 ml of isopropanol / tetrahydrofuran (5 / 2), heat to reflux for 1 hour, and heat suction filtration. After the filtrate naturally drops to room temperature, stir overnight at 0°C for crystallization, suction filtration, The filter cake was washed with a small amount of ethanol to obtain 8.5 g of white crystals, namely isopamicin benzyl ether crystal...

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Abstract

The invention provides a refining method of isepamicin. The method comprises the steps as follows: S1, a crude isepamicin product is subjected to a benzyl protection reaction to form benzyl isepamicin; S2, the benzyl isepamicin prepared in S1 is dissolved by a solvent and recrystallized to obtain benzyl isepamicin crystals; S3, the benzyl isepamicin crystals prepared in S2 are subjected to a deprotection reaction to prepare a target product isepamicin. According to the refining method of isepamicin, the crude isepamicin product can be refined and purified with a simple chemical method, the refinement and purification process of isepamicin is simplified, the product stability is good, and the method is suitable for industrial mass production.

Description

technical field [0001] The invention belongs to the technical field of biomedicine, and more specifically relates to a method for refining isopamicin. Background technique [0002] Isopamicin is the 1-position C atom NH of gentamicin B 2 Semi-synthetic aminoglycosides with the isoserinyl group. Similar to other aminoglycosides, its antibacterial mechanism is to inhibit bacterial protein synthesis by acting on ribosomes in bacteria, and destroy the integrity of bacterial cell membranes, resulting in the destruction of bacterial cell membranes and cell death. The characteristic of isopamicin is that the presence of isoserinyl group strengthens the stability of inactivating enzymes to various aminoglycoside drugs, and has antibacterial activity against some strains resistant to gentamicin. Isopamicin has strong antibacterial activity against Escherichia coli, Citrobacter, Klebsiella, Enterobacter, Serratia, Proteus, Pseudomonas aeruginosa, etc. Bacteroides fragilis, Xanthomo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H1/00C07H15/236
CPCC07H1/00C07H15/236
Inventor 王涛李晓明王庆林王彬彬孙益林
Owner ZHUOHE PHARM GRP CO LTD