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Synthesis method and application of pefloxacin mesylate

A technology of pefloxacin mesylate and its synthesis method, which is applied to the preparation of sulfonate, medical preparations containing active ingredients, and pharmaceutical formulas, which can solve problems such as operator danger and equipment corrosion, and reduce the process flow , reduce corrosion, improve the effect of utilization

Pending Publication Date: 2021-07-20
CHINA MEHECO SANYANG PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Although this method does not need to produce norfloxacin, the methylation reaction of formaldehyde and formic acid that corrodes the equipment is eliminated, and the obtained intermediate crude product does not need to be refined, and can be directly put into the next step reaction, but it also needs to go through high temperature alkaline Hydrolysis, although hydrochloric acid will be used to neutralize later, under alkaline conditions, there is still a certain degree of corrosion to the equipment, and there is also a certain degree of danger to the operator

Method used

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  • Synthesis method and application of pefloxacin mesylate
  • Synthesis method and application of pefloxacin mesylate
  • Synthesis method and application of pefloxacin mesylate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Embodiment 1 A kind of synthetic method of pefloxacin mesylate A1

[0028] The present embodiment provides a kind of synthetic method of pefloxacin mesylate A1, it is

[0029] Weigh 38.3g dimethyl ((7-chloro-6-fluoro-1-methyl-4-carbonyl-1,4-dihydroquinoline-3-carbonyl) oxo) borane dicarboxylate and 10.0 Add g N-methylpiperazine to 50ml THF and stir, add 42ml TEA while stirring continuously, raise the temperature to 60°C and keep stirring for 4 hours, take a small amount of reaction solution and send it to liquid chromatography to monitor the reaction progress, the peak of the raw material disappears, which is the end of the reaction , Evaporate the residual solvent and TEA under reduced pressure, add 100ml ethanol to mix and dissolve, add 28.5g methanesulfonic acid, heat up to 90°C and continue stirring for 6h, a large amount of solid precipitates, TLC monitors the reaction, and the disappearance of the raw material point is the end of the reaction. Filter the reaction...

Embodiment 2～6

[0032] The synthetic method of embodiment 2~6 pefloxacin mesylate A2~A6

[0033] The synthesis method of pefloxacin mesylate A2-A6 provided in Examples 2-6 is basically the same as the synthesis method of pefloxacin mesylate A1 described in Example 1, the difference is that some process parameters are different, specifically The process parameters are shown in Table 1.

[0034] Table 1: Process parameter table of pefloxacin mesylate A2~A6

[0035]

[0036]

[0037] Other parameters are all the same as in Example 1.

experiment example

[0042] Experimental example Stability test of pefloxacin mesylate

[0043] Choose pefloxacin mesylate A1~A6 provided by the present invention, pefloxacin mesylate D and pefloxacin mesylate S (Rewell Biotechnology) to carry out stability comparative research test, detection standard With the standard described in "Chinese Pharmacopoeia" Part Two (p228):

[0044] Selected sample is placed 3 months under the condition of temperature 40 ℃ ± 2 ℃, relative humidity 75% ± 5%, through sampling analysis, the comparison of each index analysis result and 0 month, methanesulfonic acid cultivation provided by the present invention The related substances of flufloxacin A1~A6 increased significantly, and all other detection indexes had obvious changes. % ± 5% under the condition of instability, so the accelerated test of this condition is no longer carried out.

[0045] The selected samples were stored for 6 months at a temperature of 30°C ± 2°C and a relative humidity of 65% ± 5%. After s...

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Abstract

The invention belongs to the field of medicine synthesis, and discloses a synthesis method and application of pefloxacin mesylate. According to the synthetic method, the pefloxacin mesylate is prepared from dimethyl((7-chloro-6-fluoro-1-methyl-4-carbonyl-1,4-dihydroquinolin-3-carbonyl)oxo) borane dicarboxylate and N-methyl piperazine by adopting a one-pot method through acidic hydrolysis, so that the technological process can be further shortened, and corrosion and damage of strong base to equipment and operators are reduced. The method is suitable for synthesizing the pefloxacin mesylate, and the synthesized pefloxacin mesylate is used for preparing the pefloxacin mesylate injection.

Description

technical field [0001] The invention belongs to the field of drug synthesis, and relates to a synthesis method and application of quinolone antibacterial drugs, in particular to a synthesis method and application of pefloxacin mesylate. Background technique [0002] Pefloxacin mesylate, chemical name: 1-ethyl-6-fluoro-7-(4-methyl-1-piperazinyl)-1,4-dihydro-4-oxoquinoline-3 - Carboxylic acid monomethanesulfonate dihydrate, molecular weight: 465.49. It can treat various infections caused by pefloxacin-sensitive bacteria: urinary tract infection; respiratory tract infection; ear, nose and throat infection; gynecological and reproductive system infection; abdominal and liver and biliary system infection; bone and joint infection; skin Infection; sepsis and endocarditis; meningitis. [0003] According to the Chinese invention patent application with the application number 201210317266.X, a synthesis method of pefloxacin mesylate is disclosed, in which solid formaldehyde, formic...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D215/56A61K31/496A61P31/04C07C303/32C07C309/04
CPCC07D215/56A61K31/496A61P31/04C07C303/32C07C309/04
Inventor 邝素梅朱峰章世舜张洁程云峰张振宇梅燕羊美转
Owner CHINA MEHECO SANYANG PHARMA CO LTD
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