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Impurity of neomycin sulfate and preparation method thereof

A technology of neomycin sulfate and impurities, which is applied in the field of medicine and chemical industry, can solve problems such as not being found, and achieve the effect of guaranteeing and controlling quality and improving quality standards

Inactive Publication Date: 2020-08-21
XINYU PHARM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But so far, there is no inquiry about any reports about these two compounds

Method used

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  • Impurity of neomycin sulfate and preparation method thereof
  • Impurity of neomycin sulfate and preparation method thereof
  • Impurity of neomycin sulfate and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] Take a 50mL dry three-necked glass reaction bottle, under the protection of nitrogen, add 200mg of neomycin impurity D and 10mL of ethyl acetate solvent, stir and dissolve evenly, put it in an ice bath at 0°C, take 0.029g of acetyl chloride and dissolve it in 10mL of dry ethyl acetate The ester solution was slowly added dropwise, and the drop was completed within about 10 minutes. The reaction was maintained at this temperature for about 1 hour, and monitored by HPLC until the end. The reaction mixture was spin-dried at low temperature and separated by preparative chromatography to obtain 16.2 mg of the product with a purity of 95.9% and a yield of 8.1%.

Embodiment 2

[0045] Take a 50mL dry three-necked glass reaction bottle, under the protection of nitrogen, add 200mg of neomycin impurity D and 10mL of dry solvent ethyl acetate, stir and dissolve evenly, put it in an ice bath at 0°C, take 0.046g of acetyl chloride and dissolve it in 10mL of dry acetic acid The ethyl ester solution was slowly added dropwise, and the drop was completed within about 20 minutes, then 0.008 g of DMAP was added, and the temperature was maintained for about 3 hours, and the HPLC monitoring was completed. The reaction solvent was spin-dried at low temperature and separated by preparative chromatography to obtain 54 mg of the product with a purity of 95.9% and a yield of 27.0%.

Embodiment 3

[0047] Take a 50mL dry three-necked glass reaction bottle, under the protection of nitrogen, add 200mg of neomycin impurity D and 10mL of dry solvent acetonitrile, stir and dissolve evenly, put it in an ice bath at 10°C, take 0.029g of acetyl chloride and dissolve it in 10mL of dry acetonitrile solution, Slowly add dropwise, and finish dropping within about 20 minutes. Add 0.045 g of tetrabutylammonium bromide dropwise, and then add 0.038 g of DMAP, keep the temperature for about 3 hours, and monitor by HPLC. The reaction solvent was spin-dried at low temperature, followed by preparative chromatographic separation to obtain 87 mg of the product with a purity of 98.8% and a yield of 43.5%.

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Abstract

The invention relates to an impurity of neomycin sulfate and a preparation method thereof. The impurity of neomycin sulfate is one or a combination of two of an impurity A and an impurity B. The preparation method comprises steps: firstly, an impurity structure is speculated, then directional synthesis is carried out, detailed structure analysis is carried out on a target compound obtained throughsynthesis, the structure of the compound is confirmed, the impurity A and the impurity B can be accurately identified and massively prepared, and a good foundation is provided for quality research ofneomycin sulfate products. The invention provides the neomycin sulfate impurity and the preparation method thereof. The method is of great significance to related research of neomycin sulfate impurities; the impurity is a reliable contrast for improving the quality of neomycin sulfate drugs and solving process impurities or degradation impurities generated in neomycin sulfate synthesis and fermentation processes. The method can be used for qualitative and quantitative analysis of impurities in synthesis and fermentation of neomycin sulfate, can improve the quality standard of neomycin sulfate, effectively guarantees and controls the quality of neomycin sulfate, and has important application value for quality research and preparation research of neomycin sulfate raw materials.

Description

technical field [0001] The invention belongs to the technical field of medicine and chemical industry, and in particular relates to an impurity of neomycin sulfate and a preparation method thereof. Background technique [0002] Neomycin sulfate is an aminoglycoside antibiotic, which is a mixture isolated from the metabolites of Streptomycesfradiae in 1949. It contains three components A, B and C, of ​​which B and C are the main components. Escherichia coli, para-Escherichia coli, Pseudomonas aeruginosa, Bacillus aerogenes, Proteus vulgaris, pneumococcus, Corynebacterium diphtheriae, Neisseria meningitidis, Lactobacillus, Neisseria gonorrhoeae, Klebsiella pneumoniae, Salmonella typhi, Salmonella enteritidis Bacteria, etc. are curative. The product is very soluble in water and practically insoluble in ethanol, ether, acetone or chloroform. At present, this product is widely used as a veterinary drug and has a good market prospect. [0003] With the continuous development of...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H15/224C07H1/00
CPCC07H1/00C07H15/224
Inventor 王晓东刘健蒋祖艳刘思远李为全董想
Owner XINYU PHARM CO LTD
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