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Preparation method of flomoxef sodium

A technology of fluoxetine sodium and fluoxetal acid, which is applied in the field of preparation of fluoxetal sodium, can solve problems such as difficulty in calculating the amount of raw materials and the inability to determine the amount of sodium bicarbonate, and achieve the effect of avoiding residues

Active Publication Date: 2014-01-22
SHANGHAI LONGXIANG BIO MEDICINE DEV CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The technical problem to be solved by this invention is to overcome the report of the parameters of specific process conditions, the consumption of fluoxetal acid and sodium bicarbonate or its ratio in the literature that do not have specific process conditions in the preparation process of fluoxetal sodium in the prior art, so that technical personnel It is impossible to determine the amount of sodium bicarbonate used in actual production, and due to the influence of flumoxefolic acid and sodium bicarbonate impurities, it is difficult to calculate the actual amount of raw materials. A preparation method for fluoxefom sodium is provided

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Slowly add saturated sodium bicarbonate solution dropwise to 120 g of fluoxetal acid at a temperature of 0° C., accompanied by vigorous stirring. The stirring speed is 100 rpm, and the stirring time is 2 hours. While adding dropwise, check the pH value of the reaction solution with a pH meter. When the pH=4.2, stop the dropwise addition, and retest the pH after stirring for 10 minutes. The deviation does not exceed 0.1. Add 620 g of ethyl acetate / 2-butanone (volume ratio 1:1) mixed solvent, and stir for 15 min. Separate the liquid, take the water phase, add 12g of activated carbon, stir for 15min, and filter with suction. Take the filtrate and freeze-dry it to obtain 114.9 g of off-white crystals, which are fluoxetal sodium.

[0034] For the detection method and the result thereof of the various performances of fluoxetal sodium obtained in embodiment 1 are as follows:

[0035] Use high performance liquid chromatography (HPLC) to detect the purity of the fluoxetine sod...

Embodiment 2

[0056] At a temperature of 10°C, slowly dropwise add saturated sodium bicarbonate solution into 120 g of fluoxetal acid, accompanied by vigorous stirring, the stirring speed is 120 rpm, and the stirring time is 1.5 h. While adding dropwise, check the pH value of the reaction solution with a pH meter. When the pH=4.5, stop the dropwise addition, and retest the pH after stirring for 10 minutes. The deviation does not exceed 0.1. Add 620g of ethyl acetate / 2-butanone (1:1) mixed solvent and stir for 15min. Separate the liquid, add 12 g of activated carbon to the water phase, stir for 15 min, and filter with suction. Take the filtrate and freeze-dry it to obtain 113.5 g of off-white crystals, which are fluoxetal sodium.

[0057] The detection conditions of the various performances of the fluoxetine sodium that the preparation method of embodiment 2 makes is all the same as embodiment 1, and its detection result is: the purity of the fluoxetine sodium that makes is 99.5%; 1-hydroxy...

Embodiment 3

[0060] Slowly add saturated sodium bicarbonate solution dropwise to 120 g of fluoxetal acid at a temperature of 5° C., accompanied by vigorous stirring. The stirring speed is 100 rpm, and the stirring time is 2 hours. While adding dropwise, check the pH value of the reaction solution with a pH meter. When the pH=5.0, stop the dropwise addition, and retest the pH after stirring for 10 minutes. The deviation does not exceed 0.1. Add 620g of ethyl acetate / 2-butanone (1:1) mixed solvent and stir for 15min. Separate the liquid, add 12 g of activated carbon to the water phase, stir for 15 min, and filter with suction. Take the filtrate and freeze-dry it to obtain 115.5 g of off-white crystals, which are fluoxetal sodium.

[0061] The detection conditions of the various performances of the fluoxetine sodium that the preparation method of embodiment 3 makes is all the same as embodiment 1, and its detection result is: the purity of the fluoxefom sodium that makes is 99.3%; 1-hydroxye...

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Abstract

The invention discloses a preparation method of flomoxef sodium. The preparation method comprises the following steps of dropwise adding a sodium bicarbonate solution into flomoxef acid while stirring at the temperature of 0-10 DEG C until the pH value of a reaction solution is up to 4.2-5.2, and after flomoxef acid is completely dissolved, extracting, decoloring and removing a decolorizing agent to obtain flomoxef sodium. By using the preparation method of flomoxef sodium, provided by the invention, flomoxef sodium can be effectively and uniformly produced in real time, the residues of sodium salt and flomoxef acid in a product are avoided, the purity of obtained flomoxef sodium is larger than or equal to 99%, and the residual quantity of 1-ethoxyl-5-thiol-1H-tetrazole is smaller than or equal to 0.2%, therefore, the standard requirement of Japanese pharmacopoeia JP16 is completely met.

Description

technical field [0001] The invention relates to a preparation method of fluoxyceph sodium. Background technique [0002] Fluoxefor sodium is an oxacephalosporin antibiotic developed and marketed by Shionogi Pharmaceutical Co., Ltd. in Japan in 1988. The finished product is made into an injection in the form of sodium salt. It is very stable to lactamase, its antibacterial spectrum is similar to other third-generation cephalosporins, and its antibacterial effect on Gram-positive bacteria is almost the same as other cephalosporins. Fluoxetal has a strong antibacterial effect on Staphylococcus aureus, especially against drug-resistant Staphylococcus aureus including methicillin-resistant Staphylococcus aureus (MRSA); The clinical effect is very good, and a certain amount of fluoxetal can penetrate into the cerebrospinal fluid through the blood-brain barrier. [0003] At present, the literature reports mainly focus on the research on the synthetic route of fluoxetal acid, the ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D501/57C07D501/04
CPCC07D501/04C07D501/57
Inventor 冯虓唐方强崔英杰
Owner SHANGHAI LONGXIANG BIO MEDICINE DEV CO LTD
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