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Application of silver catalyst in preparation of antibacterial drug intermediate

A silver catalyst and antibacterial technology, applied in the field of drug synthesis, can solve the problems of high preparation cost of modified PW/C catalyst, difficult to realize industrialization, low catalytic activity, etc., and achieve shortened reaction time, simple post-processing, and high catalytic activity. Effect

Inactive Publication Date: 2021-02-26
商河探荣新技术开发中心
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, H 2 WO 4 The catalytic activity of the / C catalyst is low, and the yield of the vortex salt is only about 60%. The preparation cost of the modified PW / C catalyst is high, the process is complicated, and it is difficult to realize industrialization

Method used

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Examples

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Comparison scheme
Effect test

preparation example Construction

[0028] The invention provides a preparation method of fosfomycin left phosphorus and right ammonium salt. The preparation method comprises the following steps: at room temperature, dissolving cisacrylphosphonic acid in an alcoholic solvent, and then slowly adding (+)-α-phenylethyl ether Amine, after the dropwise addition, adjust the pH of the system to 5.5~6, continue to stir for 1~3min, then add the silver catalyst, and continue to drop hydrogen peroxide slowly. At 55°C, filter while it is hot, then cool the filtrate, crystallize, and wash to obtain fosfomycin left phosphorus and right ammonium salt.

[0029] According to the preparation method of an antibacterial drug intermediate fosfomycin levophosphine salt of the present invention, the silver catalyst is preferably silver carbonate.

[0030] According to the preparation method of an antibacterial drug intermediate fosfomycin levophosphine salt of the present invention, the alcohol solvent is selected from one or more of ...

Embodiment 1

[0043] At room temperature, dissolve 0.1mol cis-acrylphosphonic acid in absolute ethanol, then slowly add 0.11mol (+)-α-phenylethylamine dropwise, after the dropwise addition, adjust the pH of the system to 5.5, and continue stirring for 3 minutes. Then add 0.2g of silver carbonate powder, and slowly add 17g (0.15mol) of 30% hydrogen peroxide dropwise. After the dropwise addition, continue to stir for 30min. The filtrate was cooled to 0°C for crystallization, and then the crystals were washed with ice ethanol to obtain fosfomycin levophosphine salt with a yield of 94.6%.

Embodiment 2

[0045] At room temperature, dissolve 0.1mol cis-acrylphosphonic acid in absolute ethanol, then slowly add 0.15mol (+)-α-phenylethylamine dropwise, after the dropwise addition, adjust the pH value of the system to 6, and continue stirring for 3 minutes. Then add 0.5g of silver carbonate powder, and slowly add 17g (0.15mol) of 30% hydrogen peroxide dropwise. After the dropwise addition, continue to stir for 30min. The filtrate was cooled to 0°C for crystallization, and then the crystals were washed with ice ethanol to obtain fosfomycin levophosphine salt with a yield of 96.2%.

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Abstract

The invention provides an application of a silver catalyst in preparation of an antibacterial drug intermediate fosfomycin levoforight amine salt. The application is characterized by comprising the following steps: at room temperature, dissolving cis-propenylphosphonic acid in an alcohol solvent, slowly dropwise adding (+) alpha phenylethylamine, regulating the pH value of the system to 5.5-6 after dropwise adding, continuing stirring for 1-3 minutes, and adding the silver catalyst, continuously and slowly dropwise adding hydrogen peroxide, then continuously stirring for 10-30 minutes, quicklyheating the system to 50-55 DEG C, filtering while the system is hot, and cooling, crystallizing and washing the filtrate to obtain the fosfomycin levoforight amine salt. Silver carbonate is used asthe catalyst, hydrogen peroxide is used as an oxidizing agent, heating is not needed in the oxidative cyclization process, and the reaction can be performed at normal temperature. Silver carbonate hasvery high catalytic activity in the invention, and compared with the prior art, the application has the advantages of small dosage, mild reaction, effective shortening of the reaction time, simple post-treatment, and realization of separation of the catalyst from the system only through filtration of the system while the system is hot.

Description

technical field [0001] The invention belongs to the field of drug synthesis, in particular to a preparation method of an antibacterial drug intermediate, and more specifically to a preparation method of an important antibacterial drug intermediate fosfomycin levophosphine salt. Background technique [0002] Fosfomycin (phosphomyein, fosfomyein, FOM) chemical name: (1R,2S-(-)-cis-1,2-epoxypropylphosphonic acid, molecular formula: C 3 h 7 o 4 P, is an antibiotic with broad spectrum, low toxicity, less sensitization, less resistance, and synergistic effect with most antibiotics. Fosfomycin was discovered in Streptomyces in Spanish soil by Merck and CEPA in 1967. Fosfomycin has stable epoxy groups and phosphonic acid groups, and its efficacy is very stable, which is significantly different from most similar drugs. Synergistic effect, sensitive to Staphylococcus, Escherichia coli, Neisseria meningitidis, Neisseria gonorrhoeae, Salmonella typhi, Serratia, Proteus, Pseudomonas a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/655C07C211/27C07C209/68
CPCC07F9/65502C07C209/68C07C211/27
Inventor 李治泉
Owner 商河探荣新技术开发中心
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