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Preparation technology of mezlocillin sodium

A mezlocillin sodium and preparation technology, applied in the direction of organic chemistry, etc., can solve the problems of the large gap between original drugs and the large amount of impurities in mezlocillin sodium, and achieve the effect of reducing impurities and reducing side reactions

Inactive Publication Date: 2017-07-21
REYOUNG PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] The purpose of the present invention is to provide a kind of preparation technology of mezlocillin sodium, solve the problem that the amount of impurities of mezlocillin sodium prepared under the existing process conditions is large, and the gap with the original drug is large, the prepared mezlocillin sodium Compared with the original drug, it is superior to the original drug in terms of impurities

Method used

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  • Preparation technology of mezlocillin sodium
  • Preparation technology of mezlocillin sodium
  • Preparation technology of mezlocillin sodium

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] The preparation technology of mezlocillin sodium comprises the following steps:

[0028] (1) Add 180mL of purified water to a 1000mL three-neck flask, control the temperature at 5°C, add 20g of ampicillin trihydrate, add triethylamine to adjust the pH to 9.5, dissolve it, add 6.0g of 1-chloroformyl-3- The mixture of methylsulfonyl-2-imidazolidinone and 100mL ethyl acetate was controlled at a temperature of 5°C, and the dropwise addition time was 30min, 6.0g of sodium bicarbonate was added, stirred for 15min, and then 6.0g of 1-chloroformyl - Add the mixture of 3-methylsulfonyl-2-imidazolidinone and 100mL ethyl acetate dropwise to the above solution for 120min, control the pH to 7.2, and react for 30min after the dropwise addition, add 1g of activated carbon to the feed solution to decolorize 30min, temperature 5°C, filter;

[0029] (2) Raise the temperature of the feed solution to 19°C, add hydrochloric acid with a volume concentration of 4mol / L to acidify to pH 1.2, l...

Embodiment 2

[0031] The preparation technology of mezlocillin sodium comprises the following steps:

[0032] (1) Add 180mL of purified water to a 1000mL three-neck flask, control the temperature at 2°C, add 20g of ampicillin trihydrate, add triethylamine to adjust the pH to 9.0, dissolve it, add 6.0g of 1-chloroformyl-3- The mixture of methylsulfonyl-2-imidazolidinone and 100mL ethyl acetate was controlled at a temperature of 2°C, and the dropwise addition time was 30min. Added 5.5g of sodium bicarbonate, stirred for 15min, and then added 6.5g of 1-chloroformyl - Add the mixture of 3-methylsulfonyl-2-imidazolidinone and 100mL ethyl acetate dropwise to the above solution for 120min, control the pH to 6.8, and react for 30min after the dropwise addition, add 1g of activated carbon to the feed solution to decolorize 30min, temperature 2°C, filter;

[0033] (2) Raise the temperature of the feed solution to 16°C, add hydrochloric acid with a volume concentration of 4mol / L to acidify to a pH of...

Embodiment 3

[0035] The preparation technology of mezlocillin sodium comprises the following steps:

[0036] (1) Add 180mL of purified water to a 1000mL three-neck flask, control the temperature at 4°C, add 20g of ampicillin trihydrate, add triethylamine to adjust the pH to 8.7, dissolve it, add 6.3g of 1-chloroformyl-3- The mixture of methylsulfonyl-2-imidazolidinone and 100mL ethyl acetate was controlled at a temperature of 4°C, and the dropwise addition time was 40min. Added 5.0g of sodium bicarbonate, stirred for 15min, and then added 6.7g of 1-chloroformyl - Add the mixture of 3-methylsulfonyl-2-imidazolidinone and 100mL ethyl acetate dropwise to the above solution for 100min, control the pH to 7.0, and react for 30min after the dropwise addition, add 1g of activated carbon to the feed solution for decolorization 30min, temperature 4°C, filter;

[0037] (2) Raise the temperature of the feed solution to 18°C, add hydrochloric acid with a volume concentration of 4mol / L to acidify to pH...

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Abstract

The invention relates to a preparation technology of mezlocillin sodium, and belongs to the technical field of drug synthesis. The preparation technology comprises the steps of performing an acylation reaction on ampicillin trihydrate and 1-chloroformyl-3-mesyl-2-imidazolidinone under a low-temperature alkaline condition, performing decoloration, filtering, acidification, washing and dehydration, adding sodium salt, and then performing crystallization to obtain mezlocillin sodium, wherein ampicillin needs to be dissolved and clarified by triethylamine prior to the acylation reaction; and 1-chloroformyl-3-mesyl-2-imidazolidinone and an ethyl acetate solvent are mixed and then added to a reaction system twice. According to the preparation technology, a dissolution manner of ampicillin trihydrate is changed and an addition manner of 1-chloroformyl-3-mesyl-2-imidazolidinone is changed, so that a side reaction in a reaction process is reduced; the washing is performed by purified water after the acidification and anhydrous sodium acetate is used during the crystallization, so that impurities are further reduced; compared with an original drug, a prepared product has the advantages in the quantity and levels of the impurities.

Description

technical field [0001] The invention relates to a preparation process of mezlocillin sodium, which belongs to the technical field of medicine synthesis. Background technique [0002] Mezlocillin sodium is a broad-spectrum semi-synthetic penicillin antibiotic, and its molecular structure is as follows: [0003] [0004] The medicinal form of mezlocillin sodium is an injection, which was developed by Bayer AG of Germany. It was first launched in Germany in 1977. It was officially approved by the US FDA in 1981 and launched in the United States. Since the 1980s, it has been successively sold in the United States, Japan, Italy, and the Netherlands , Switzerland, China and other countries listed. At present, there are about 16 manufacturers of mezlocillin sodium raw materials in China. The synthesis process mainly uses ampicillin trihydrate and 1-chloroformyl-3-methylsulfonyl-2-imidazolidinone to prepare mezlocillin through condensation reaction. Xilin, and sodium salt (sodi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D499/68C07D499/16
CPCC07D499/68C07D499/16
Inventor 苗得足高峰刘立强刘海峰
Owner REYOUNG PHARMA
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