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Method for purifying cefotetan disodium

A technology of cefotetan disodium and a purification method, which is applied in the field of chemical pharmacy, can solve the problems of high isomer content of cefotetan disodium, achieve the effects of simplifying the production process and reducing production costs

Inactive Publication Date: 2013-04-17
SHENZHEN CHINA RESOURCES GOSUN PHARMA CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] In view of this, the present invention provides a method for purifying cefotetan disodium to solve the problem of excessive cefotetan disodium isomer (II) content in the cefotetan disodium crude product prepared in the prior art

Method used

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  • Method for purifying cefotetan disodium
  • Method for purifying cefotetan disodium
  • Method for purifying cefotetan disodium

Examples

Experimental program
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Embodiment 1

[0039] At 0-5°C, add 50g of cefotetan disodium crude product (the content of isomers detected by HPLC is (3.55%)) into 180mL of water to dissolve completely, and add 0.38g of anhydrous calcium chloride ( The molar ratio to the isomer is 1.2:1) dissolved in 5mL of water, and at 0-5°C, add the calcium chloride aqueous solution to the cefotetan disodium aqueous solution within 30 minutes. Stir for 60 minutes, filter, wash the precipitate with 10mL of water, and combine the filtrates (the content of isomers detected by HPLC is 0.01%);

[0040] At 0-5°C, add the filtrate dropwise to 2000mL of absolute ethanol for crystallization within 60 minutes. After the dropwise addition, grow the crystals at the same temperature for 60 minutes, filter, wash with acetone 200mLx3, drain, and transfer the product to Put it into the desiccator, and use the method of gradient temperature to dry the product, that is, under the vacuum pressure greater than 0.98MPa, dry at a drying temperature of 25°C...

Embodiment 2

[0041] Example 2Ca 2+ Effect of ion dosage on isomers and yields.

[0042] According to the preparation method of embodiment 1, adopt different Ca 2+ Purification of Cefotetan Disodium Crude by Ion Dosage In addition to Ca 2+ Except ion consumption, other reactant and content are identical with embodiment 1, and experimental result is as shown in table 1 below:

[0043] Table 1: Different Ca 2+ Experimental results of ion dosage:

[0044]

[0045] From the above results, it can be seen that: Ca 2+ The ion can effectively remove the isomers of cefotetan disodium, and its dosage has a great influence on the content of the isomers of cefotetan disodium and the yield of the product. If the dosage is small, the isomers cannot be completely removed. A part of cefotetan disodium will also precipitate out, which has a greater impact on the yield. Moreover, the isomer content in the crude product of cefotetan disodium has no clear impact on product quality, as long as the corre...

Embodiment 3

[0046] Example 3 Effect of Gradient Heating on Isomer Content.

[0047] According to the preparation method of Example 1, different gradient heating curves are adopted, wherein except that the heating curve is different during drying, other reactants and contents are the same as in Example 1, and the experimental results are shown in Table 2 below:

[0048] Table 2: Experimental results of different heating schemes:

[0049]

[0050]

[0051] From the above results, it can be seen that the heating curves made from different heating schemes are different. To achieve qualified moisture, the drying time is quite different, and the isomer content difference after drying is also relatively large. Comprehensive the above schemes , heating curve 4 is more suitable for process requirements.

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Abstract

The invention suitable for the field of chemical pharmacy provides a method for purifying cefotetan disodium. The method comprises the steps as follows: providing raw materials; depositing; removing impurities; filtering; and drying. According to the method, crude cefotetan disodium is reacted with calcium salt, and cefotetan disodium isomers (II) are reacted with calcium ions to generate deposits, so that the cefotetan disodium isomers (II) are greatly reduced; and meanwhile, purified cefotetan disodium is obtained in combination with a solvent-out crystallization method, so that the production process is simplified and the production cost is reduced.

Description

technical field [0001] The invention belongs to the field of chemical pharmacy, in particular to a method for purifying cefotetan disodium. Background technique [0002] Cefotetan disodium is a cephamycin, its effect is similar to that of the third-generation cephalosporins, and its antibacterial spectrum is expanded compared with that of the second-generation. And some Bacteroides fragilis are effective. It is invalid for Streptococcus faecalis and Clostridium difficile. Enzyme resistance is strong, and for some Gram-negative strains resistant to the first or second generation cephalosporins, the third generation cephalosporins are often effective. It has a good effect on enzyme-producing Gram-negative bacteria and anaerobic bacteria. [0003] The preparation method of cefotetan disodium is generally as follows: the reaction condition is at -5~0°C, the pH value of the reaction system is adjusted between 6.5~8.5 with CO2, and the isomer detected by HPLC is lower than 1%, ...

Claims

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Application Information

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IPC IPC(8): C07D501/57C07D501/12
Inventor 高顺清蒋雄杰黄权华张远杏苏军权易夏赖宝林
Owner SHENZHEN CHINA RESOURCES GOSUN PHARMA CO LTD
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