Cefamandole nafate refining method

A technology of cefamandole sodium and a refining method, which is applied in the refining field of cefamandole sodium, can solve the problems of low yield and cannot be completely solved, and achieves the effects of high purity, stable product quality and good stability

Inactive Publication Date: 2016-06-29
顾伟
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Patent CN201310011433.2 adopts mixed organic solvent as poor solvent and injection water as good solvent to obtain cefamandole sodium product with better color and higher purity, but the yield is lower
[0007] Although the purification methods disclosed in the prior art can solve the above-mentioned color and purity problems to a certain extent, they still cannot completely solve the problems

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] A, polyvinylpyrrolidone is dissolved in the mixed solvent of methanol:water=5:1, is made into 0.2mol L -1 30ml of polyvinylpyrrolidone solution, then add cefamandole sodium crude product 10g (cefamandolate sodium content is 89%, free acid content is 5.5%), be heated to 50 ℃, after dissolving completely, add activated carbon, stir 10min Afterwards, filter to obtain the filtrate for subsequent use;

[0027] B, in the filtrate of step A, dropwise add 15% sodium isooctanoate, adjust pH to 6.5, obtain cefamandole sodium crude product solution;

[0028] C, under stirring, add 30ml of acetone dropwise to the crude product solution of cefamandole sodium described in step B, dropwise, ultrasonic 10min, continue to add acetone 30ml, stir at room temperature for 2h, precipitate a large amount of crystals, filter, use a small amount of ethanol After washing and drying in vacuo, 9.19 g of fine cefamandole sodium was obtained (91.9% yield).

[0029] Detection: the color grade is No...

Embodiment 2

[0031] A, polyvinylpyrrolidone is dissolved in ethanol: in the mixed solvent of water=4:1, is made into 0.3mol L -1 40ml of polyvinylpyrrolidone solution, then add cefamandole sodium crude product 10g (cefamandolate sodium content is 89%, free acid content is 5.5%), be heated to 80 ℃, after dissolving completely, add activated carbon, stir 30min Afterwards, filter to obtain the filtrate for subsequent use;

[0032] B, in the filtrate of step A, dropwise add 15% sodium isooctanoate, adjust pH to 7.0, obtain cefamandole sodium crude product solution;

[0033] C, under stirring, add 40ml of acetone dropwise to the cefamandole sodium crude product solution described in step B, dropwise, ultrasonic 10min, continue to add acetone 40ml, stir at room temperature for 1.5h, precipitate a large amount of crystals, filter, use a small amount of Washed with ethanol and dried in vacuo to obtain 9.42 g of fine cefamandole sodium (yield 94.2%).

[0034] Detection: the color grade is less th...

Embodiment 3

[0036] A. Dissolve polyvinylpyrrolidone in a mixed solvent of isopropanol: water = 3:1 to make 0.4mol L -1 50ml of polyvinylpyrrolidone solution, then add cefamandole sodium crude product 10g (cefamandolate sodium content is 89%, free acid content is 5.5%), be heated to 65 ℃, after dissolving completely, add activated carbon, stir 30min Afterwards, filter to obtain the filtrate for subsequent use;

[0037] B, in the filtrate of step A, drip 15% sodium isooctanoate, adjust pH to 6.8, obtain cefamandole sodium crude product solution;

[0038] C, under stirring, add 35ml of acetone dropwise to the crude product solution of cefamandole sodium described in step B, dropwise, ultrasonic 30min, continue to add acetone 35ml, stir at room temperature for 2h, precipitate a large amount of crystals, filter, use a small amount of ethanol After washing and vacuum drying, 9.28 g (92.8%) of fine cefamandole sodium was obtained.

[0039] Detection: the color grade is No. 1, the HPLC purity i...

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Abstract

The invention provides a cefamandole nafate refining method. The method comprises the steps of A, dissolving polyvinylpyrrolidone in a lower alcohol and water mixed solvent to prepare a polyvinylpyrrolidone solution of 0.1-1.0 mol / L, then adding a cefamandole nafate crude product, increasing temperature to 50-80 DEG C, adding activated carbon after complete dissolution, conducting stirring for 10-30 min, and then conducting filtration to obtain a filtrate for use; B, adding sodium iso-octoate of 15% to the filtration obtained in the step A dropwise, and regulating pH to 6.0-7.0, so that a cefamandole nafate crude product solution is obtained; C, adding acetone to the cefamandole nafate crude product solution obtained in the step B dropwise while stirring, then conducting ultrasonic treatment for 10-30 min, continuing to add acetone, conducting stirring at indoor temperature for 1-2 h to enable a large number of crystals to be separated out, conducting filtration, conducting washing with a small amount of ethyl alcohol, and conducting vacuum drying so that a cefamandole nafate refined product can be obtained, wherein the amount of acetone added at the second time is 0.8-1.2 times that of acetone added at the first time. The refining method has the advantages that yield and purity are high, and the product is high in stability and light in color.

Description

technical field [0001] The invention relates to a processing method of cefamandole sodium, in particular to a refining method of cefamandole sodium. Background technique [0002] Cefamandole sodium (Cefamandol Nafate) is a second-generation cephalosporin antibiotic, which was successfully developed by E.Lilly Company of the United States at first, and its chemical name is: 7-D-(2-formyloxyphenylacetamide)-3-[ (1-Methyl-1H-tetrazol-5-yl)mercaptomethyl]-3-cephem-4-carboxylic acid sodium salt. Molecular formula is C 19 h 17 N 6 NaO 6 S 2 , the molecular weight is 512.50, the CAS number is: 30034-03-8, and the structural formula is as follows: [0003] [0004] Cefamandole sodium is a cephalosporin with strong bactericidal effect. It has the advantages of the first-generation and third-generation cephalosporins. It is effective against most Gram-positive bacteria and some Gram-negative bacteria. Bacillus has strong antibacterial activity, especially against influenza b...

Claims

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Application Information

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IPC IPC(8): C07D501/36C07D501/12
CPCC07D501/36C07D501/12
Inventor 顾伟
Owner 顾伟
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