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Cefetamet pivoxil hydrochloride compound and preparation method thereof

A technology for ceftazime pivoxil hydrochloride and a compound, which is applied in the refining field of ceftazidime pivoxil hydrochloride compounds, can solve the problems of difficulty in preparing preparations, unattainable preparations, low purity of cefetamet pivoxil hydrochloride, etc., and achieves low cost , improve the quality, the effect of convenient operation

Inactive Publication Date: 2009-10-07
郑仙锋
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The purity of the ceftazidime pivoxil hydrochloride prepared by this method is relatively low, and it cannot reach the limit required by the preparation standard, so it is difficult to prepare a qualified preparation, and the general dissolution and crystallization refining method cannot fundamentally improve its purity

Method used

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  • Cefetamet pivoxil hydrochloride compound and preparation method thereof
  • Cefetamet pivoxil hydrochloride compound and preparation method thereof

Examples

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Effect test

Embodiment 1

[0020] (1) Dissolve 100 g of ceftazidime pivoxil hydrochloride crude product in 600 ml of methanol, add 230 ml of 2 mol / L sodium hydroxide solution, stir and react at room temperature for 60 minutes, hydrolyze to separate crystals, filter, wash with water, and dry under reduced pressure at 50°C , to obtain 95.4 g of cefetamet sodium salt, with a yield of 95.4%;

[0021] (2) Dissolve cefetamet sodium salt in 800ml of water, add 8g of activated carbon for adsorption for 30 minutes, filter and decarburize, then add 88.3g of iodomethyl pivalate and 300ml of N,N-dimethylformamide, and stir at room temperature for reaction After 60 minutes, add 600ml of ethyl acetate and 100ml of water, stir and extract, separate layers, wash the organic phase with 400ml of water and saturated sodium carbonate solution, then dry with anhydrous sodium sulfate, filter, concentrate under reduced pressure, and evaporate the organic solvent , and dried under reduced pressure at 50° C. to obtain 89.5 g of...

Embodiment 2

[0024] (1) Dissolve 100 g of ceftazidime pivoxil hydrochloride crude product in 800 ml of ethanol, add 250 ml of 2 mol / L potassium hydroxide solution, stir and react at room temperature for 60 minutes, hydrolyze to separate crystals, filter, wash with water, and dry under reduced pressure at 50°C , to obtain 96.7g of cefetamet potassium salt, with a yield of 96.7%;

[0025] (2) Dissolve cefetamet potassium salt in 1000ml of water, add 10g of activated carbon for adsorption for 30 minutes, filter for decarburization, then add 102.2g of iodomethyl pivalate and 500ml of N,N-dimethylsulfoxide, and stir at room temperature for reaction After 60 minutes, add 800ml of ethyl acetate and 200ml of water, stir and extract, separate layers, wash the organic phase with 600ml of water and saturated sodium carbonate solution, then dry with anhydrous magnesium sulfate, filter, concentrate under reduced pressure, and evaporate the organic solvent , dried under reduced pressure at 50° C. to obt...

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Abstract

The invention discloses a cefetamet pivoxil hydrochloride compound and a preparation method thereof. In the method, the crude product of cefetamet pivoxil hydrochloride prepared by the prior art is processed by the following steps to obtain a relatively pure cefetamet pivoxil hydrochloride compound: the crude product of cefetamet pivoxil hydrochloride is dissolved in methanol or alcohol, and then sodium hydroxide solution or potassium hydroxide solution is added; the mixed solution is stirred for reaction and hydrolyzed to obtain cefetamet pivoxil sodium salt or cefetamet pivoxil sylvite which is then absorbed with added active carbon and filtered; and then iodo-ester is added and reaction is conducted in the presence of an organic solvent to obtain cefetamet pivoxil; the cefetamet pivoxil dissolves in isopropyl alcohol, hydrochloric acid is added in a dropwise manner and cyclohexane is added, and the mixed solution is stirred to separate out crystal; and the crystal is filtered, washed and dried to obtain cefetamet pivoxil hydrochloride.

Description

technical field [0001] The invention relates to a method for refining ceftamet pivoxil hydrochloride compound, which belongs to the technical field of medicine. Background technique [0002] Ceftazidime pivoxil hydrochloride, its chemical name is: (6R, 7R)-3-methyl-7-[(Z)-2-(2-amino-4-thiazolyl)-2-(methoxyimino) -Acetamido]-8-oxo-5-thia-1-azabicyclo[4,2,0]oct-2-ene-2-carboxylic acid pivaloyloxymethyl ester hydrochloride, molecular formula: C 20 h 25 N 5 o 7 S 2 HCl, molecular weight: 548.04, structural formula: [0003] [0004] Oral third-generation broad-spectrum cephalosporin antibiotics have strong antibacterial activity against both Gram-positive and Gram-negative bacteria, and are stable against β-lactamase produced by bacteria. It is clinically applicable to lower respiratory tract infection, ear, nose, throat infection and urinary system infection caused by sensitive bacteria. [0005] About the synthetic method of ceftazidime pivoxil hydrochloride, in "Jou...

Claims

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Application Information

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IPC IPC(8): C07D501/22C07D501/12A61P31/04
Inventor 郑仙锋
Owner 郑仙锋
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