Preparation method for Azlocillin sodium

A technology of azlocillin sodium and ampicillin, applied in the field of antibiotic drug synthesis, can solve the problems of large amount of chemical solvent used, affecting product yield, loss of chromatographic operation, etc., to reduce the risk of degradation in the presence of alkali, and easy to operate , the effect of reducing risk

Active Publication Date: 2012-01-11
JIANGSU HI STONE PHARMA
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Problems solved by technology

[0008] Typical bibliographical reports are such as: "A kind of preparation method of azlocillin sodium" recommended by the invention patent authorization announcement number CN1305874C. Because the method adopts a solvent crystallization process, it needs to cooperate with ethyl acetate and ethanol as a solvent for crystallization operation, so that Troublesome operation, large amount of chemical solven

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  • Preparation method for Azlocillin sodium

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Embodiment 1

[0032] A) prepare the condensation reaction liquid, pump 1 part of dichloromethane into the reaction tank (also called the reaction tank) by weight parts, then drop into 0.075 parts (weight parts) of ampicillin in the reaction tank under stirring state, then Open the jacket of the reaction tank and cool the frozen brine to 0°C, adjust the pH to weakly alkaline with a pH adjuster, i.e. triethylamine, that is, adjust the pH to 8.0 to obtain a solution for condensation reaction;

[0033] B) Condensation reaction, first put 1-chloroformyl-2-imidazolidinone and dichloromethane into the dissolving tank and dissolve to form a mixed solution, then the mixed solution is added dropwise and within 45min to Condensation reaction is carried out in the condensation reaction solution in the reaction tank described in step A), the temperature of the condensation reaction is 10 ° C, after the dropwise addition of the aforementioned 1-chloroformyl-2-imidazolidinone and dichloromethane After the...

Embodiment 2

[0042] A) prepare the condensation reaction liquid, pump 1 part of dichloromethane into the reaction tank (also called the reaction tank) by weight parts, then drop into 0.074 parts (weight parts) of ampicillin in the reaction tank under stirring state, then Open the jacket of the reaction tank and cool the frozen brine to 5°C, adjust the pH to weakly alkaline with a pH adjuster, i.e. triethylamine, that is, adjust the pH to 7.5 to obtain a solution for condensation reaction;

[0043] B) Condensation reaction, first put 1-chloroformyl-2-imidazolidinone and dichloromethane into a dissolving tank to dissolve and form a mixed solution, then drop the mixed solution to The condensation reaction is carried out in the condensation reaction solution in the reaction tank described in step A), the temperature of the condensation reaction is 5 ° C, after the dropwise addition of the aforementioned 1-chloroformyl-2-imidazolidinone and dichloromethane After the mixed solution of the mixed ...

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Abstract

The invention relates to a preparation method for Azlocillin sodium, which belongs to the synthetic technical field of antibiotics. The preparation method comprises the following steps: preparing a solution used for a condensation reaction, drawing dichloromethane into a reactor, putting ampicillin into the reactor with stirring, controlling the weight ratio of dichloromethane to ampicillin, thencooling and controlling the reduced temperature, then regulating the pH value to alkalescence by a pH regulator to obtain an solution used for condensation reaction; performing a condensation reaction; extracting and separating; crystallizing; drying; performing a salifying reaction; decoloring; freezing and drying; crushing. The invention has the advantages that the preparation method is capableof simplifying the operation, reducing the usage of the chemical solutions and the risks on environmental pollution; and has simple operation; can effectively avoid the loss caused by chromatography,raise the yield of Azlocillin sodium; and has mild salifying reaction condition, reduce the risk that Azlocillin sodium can be decomposed in alkali. The content of a single impurity of the obtained Azlocillin sodium dried product is lower than 0.6 percent and the content of total impurity of the obtained Azlocillin sodium dried product is lower than 1 percent which are obviously superior to the pharmacopoeia standard.

Description

technical field [0001] The invention belongs to the technical field of synthesis of antibiotic drugs, and in particular relates to a preparation method of azlocillin sodium. Background technique [0002] Azlocillin sodium (English name: Azlocillin Sodium), its chemical name is: (2S, 5R, 6R)-3,3-dimethyl-6-[(R)-2-(2-oxo-1 -imidazolidinecarboxamido)-2-phenylacetamido]-7-oxo-4-thia-1-azabicyclo[3,2,0]heptane-2-carboxylic acid sodium salt. [0003] [0004] Molecular formula: C 20 h 22 N 5 NaO 6 S [0005] Molecular weight: 483.47 [0006] Azlocillin sodium was first developed by Bayer Company of Germany, and it went on the market in May 1977. Since the 1980s, it has been used in the United States, Britain and other countries. In 1983, it was included in the supplementary volume of the 20th edition of the US Pharmacopoeia. It is still recorded that its bactericidal effect on Pseudomonas aeruginosa is about ten times greater than that of carbenicillin, and it also has t...

Claims

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Application Information

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IPC IPC(8): C07D499/68C07D499/16
Inventor 王多平
Owner JIANGSU HI STONE PHARMA
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