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A kind of preparation method of cefdinir impurity m

A technology of cefdinir and impurity, which is applied in the field of preparation of cefdinir impurity M, can solve problems such as uneven quality, and achieve the effect of fewer process steps, mild reaction conditions and easy operation

Active Publication Date: 2019-01-04
PI & PI BIOTECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Throughout the domestic raw material manufacturers, there is a situation of uneven quality, good and bad

Method used

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  • A kind of preparation method of cefdinir impurity m
  • A kind of preparation method of cefdinir impurity m
  • A kind of preparation method of cefdinir impurity m

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] A preparation method of cefdinir impurity M, comprising the following steps:

[0027] (1) Weigh 10 g of cefdinir raw material, add 20 mL of sulfuric acid, stir and react for 50 h at room temperature at 30° C., to obtain a mixed solution containing cefdinir impurity M;

[0028] (2) Take 1L of the mixed solution containing cefdinir impurity M obtained in step (1), slowly add 700mL of 10% aqueous sodium hydroxide solution, stir to adjust the pH value of the mixed solution to 2.5~3.0, separate with C18 column, and use 1% , 3%, 6%, 9%, 12% acetonitrile solution elution, HPLC detection, collect 9%, 12% acetonitrile elution part, vacuum pump out acetonitrile and then use C18 column to separate, use 3 times column volume 3 times successively %, 6%, 9%, and 12% of acetonitrile aqueous solution to obtain cefdinir impurity M with a yield of 1.5% and a purity of more than 95%.

Embodiment 2

[0030] A preparation method of cefdinir impurity M, comprising the following steps:

[0031] (1) Weigh 10 g of cefdinir raw material, add 35 mL of sulfuric acid, stir and react for 35 h at room temperature at 32° C., to obtain a mixed solution containing cefdinir impurity M;

[0032] (2) Take 1L of the mixed solution containing cefdinir impurity M obtained in step (1), slowly add 700mL of 10% aqueous sodium hydroxide solution, stir to adjust the pH value of the mixed solution to 2.5~3.0, separate with C18 column, and use 1% , 3%, 6%, 9%, 12% acetonitrile solution elution, HPLC detection, collect 9%, 12% acetonitrile elution part, vacuum pump out acetonitrile and then use C18 column to separate, use 3 times column volume 3 times successively %, 6%, 9%, and 12% of acetonitrile aqueous solution to obtain cefdinir impurity M with a yield of 2.3% and a purity of over 95%.

Embodiment 3

[0034] A preparation method of cefdinir impurity M, comprising the following steps:

[0035] (1) Weigh 10 g of cefdinir raw material, add 50 mL of sulfuric acid, and stir at room temperature for 20 h at 35° C. to obtain a mixed solution containing cefdinir impurity M;

[0036] (2) Take 1L of the mixed solution containing cefdinir impurity M obtained in step (1), slowly add 700mL of 10% aqueous sodium hydroxide solution, stir to adjust the pH value of the mixed solution to 2.5~3.0, separate with C18 column, and use 1% , 3%, 6%, 9%, 12% acetonitrile solution elution, HPLC detection, collect 9%, 12% acetonitrile elution part, vacuum pump out acetonitrile and then use C18 column to separate, use 3 times column volume 3 times successively %, 6%, 9%, and 12% of acetonitrile aqueous solution to obtain cefdinir impurity M with a yield of 3.1% and a purity of over 95%.

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Abstract

The invention discloses a preparation method of a cefdinir impurity M. The preparation method comprises the steps that a cefdinir raw material reacts under the catalytic action of acid to obtain the cefdinir impurity M. The preparation method of the cefdinir impurity M is mild in condition, simple in process, easy to operate and suitable for laboratory or large-scale industrial production.

Description

technical field [0001] The invention belongs to the field of medicinal chemistry, in particular to a preparation method of cefdinir impurity M. Background technique [0002] Cefdinir (Cefdinir) belongs to the third-generation cephalosporin, and is a cephalosporin antibiotic developed by Fujisawa Pharmaceutical Co., Ltd. in Japan. It was first listed in Japan in October 1991. The trade name is Cefzon. It was listed in the United States in December 1997. It was launched in South Korea in 2001, and domestic cefdinir was approved to be listed in China in 2001. In April 2009, Shanghai Anhante Biomedical Technology Co., Ltd. applied for the import of raw materials and was approved by SFDA. Cefdinir is stable against β-lactamase, has a broad antibacterial spectrum, strong antibacterial effect, high clinical efficacy, low toxicity, less allergic reactions, and is convenient to use. Compared with drugs such as cefixime, cefuroxime, cefaclor and cefprozil, it has the strongest antiba...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D501/00C07D501/10C07D501/12
CPCC07D501/00C07D501/10C07D501/12
Inventor 袁晓林顺权欧洁梅李金菊
Owner PI & PI BIOTECH