Refinement method of cefditoren pivoxil

A technology of cefditoren pivoxil and a refining method, which is applied in the field of medicine, can solve the problems of high impurity content of cefditoren pivoxil E isomer, low purity of cefditoren pivoxil crude product, non-compliance with USP API standards, etc. , to achieve the effect of simple operation and high refining efficiency

Active Publication Date: 2016-11-16
REYOUNG PHARMA
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] For the post-treatment method of the compound of formula (3), the patent WO2005016936 adopts the solvent crystallization method to obtain the crude product of formula (3), but the crude product of cefditoren pivoxil obtained by this method has a low purity (96.8%), and cefditoren pivoxil The impurity content of E isomer is relatively high (0.78%), which does not meet the USP raw material drug standard of this variety

Method used

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  • Refinement method of cefditoren pivoxil

Examples

Experimental program
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Effect test

Embodiment 1

[0029] (1) Synthesis of crude cefditoren pivoxil

[0030] Dissolve 100g compound (1) in 1L dimethyl sulfoxide, lower the temperature to 0°C, add compound (2) dropwise, control the temperature for 1 hour, add 500mL ethyl acetate and 300mL purified water, separate the organic phase, Concentrate and crystallize at ℃ to obtain crude compound (3).

[0031] (2) Refining of crude cefditoren pivoxil

[0032] Dissolve the crude cefditoren pivoxil in 4V / W dimethyl sulfoxide, add ethyl acetate-purified water, extract, concentrate the ethyl acetate phase under reduced pressure at 40°C to 1 / 4V, stir and crystallize 3 Hours; suction filtration, add ethanol to the filter cake, stir at 60°C for 30 minutes, suction filtration, and dry under reduced pressure to obtain a light yellow powder, namely cefditoren pivoxil finished product, purity: 99.2% (plus the main component of the correction factor Self-control method). The proton nuclear magnetic resonance spectrum of cefditoren pivoxil is shown in ...

Embodiment 2

[0037] (1) Synthesis of crude cefditoren pivoxil

[0038] Dissolve 500g of compound (1) in 2L of N,N-dimethylformamide, lower the temperature to -10°C, add compound (2) dropwise, control the temperature and react for 2 hours, add 1L ethyl acetate and 1L purified water, and separate , The organic phase was concentrated and crystallized at 50°C to obtain crude compound (3).

[0039] (2) Refining of crude cefditoren pivoxil

[0040] Dissolve the crude cefditoren pivoxil in 4V / WN,N-dimethylformamide, add ethyl acetate-purified water, extract, and concentrate the ethyl acetate phase at 30°C under reduced pressure to 1 / 4V, and stir Crystallize for 2 hours; filter with suction, add ethanol to the filter cake, stir at 60°C for 20 minutes, filter with suction, and dry under reduced pressure to obtain a light yellow powder, namely the finished product of cefditoren pivoxil, purity: 98.2% (plus correction factor Principal component self-control method).

Embodiment 3

[0042] (1) The synthesis of crude cefditoren pivoxil is the same as in Example 1.

[0043] (2) Refining of crude cefditoren pivoxil

[0044] The crude cefditoren pivoxil of formula (3) was completely dissolved in 4V / WN,N-dimethylformamide, ethyl acetate-purified water was added, extraction, and the ethyl acetate phase was concentrated under reduced pressure at 40°C to 1 / 2V, stirring and crystallization for 2 hours; suction filtration, adding ethanol to the filter cake, stirring at room temperature for 30 minutes, suction filtration, and drying under reduced pressure to obtain a pale yellow powder, the finished product of cefditoren pivoxil, purity: 97.3% ( Principal component self-control method with correction factor).

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Abstract

The present invention belongs to the technical field of medicine, and particularly relates to a refinement method of cefditoren pivoxil, wherein a cefditoren pivoxil crude product is sequentially subjected to dissolution, extraction, concentration crystallization and slurry beating to finally obtain the cefditoren pivoxil pure product. According to the present invention, the current situations of poor purification effect of the cefditoren pivoxil crude product and high dimer content in the existing refinement process can be overcome, and the refinement method has advantages of simple operation and high refinement efficiency, and is suitable for large-scale industrial production.

Description

Technical field [0001] The invention belongs to the technical field of medicine, and specifically relates to a method for refining cefditoren pivoxil. Background technique [0002] Cefditoren Pivoxil is the fourth-generation cephalosporin developed by Japan Meiji Confectionery Co., Ltd., and it has obtained an import license in my country in September 2000. Cefditoren pivoxil is a prodrug of cefditoren. After oral administration, it is deesterified by intestinal wall deesterase when absorbed in the gastrointestinal tract and degraded into the active body cefditoren in vivo to show antibacterial activity. Cefditoren is a new generation of oral cephalosporins with a broad antibacterial spectrum against gram-positive and gram-negative bacteria. [0003] Compared with other similar preparations, cefditoren pivoxil has excellent antibacterial activity against pneumococcal and throphilus influenzae, and also shows strong antibacterial activity against various resistant strains. Therefor...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D501/12C07D501/56
CPCC07D501/12C07D501/56
Inventor 苗得足高峰毛可彬甄志彬张翔
Owner REYOUNG PHARMA
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