Method for converting cefotaxime acid into sodium salt crystal

A technology of cefotaxime acid and sodium salt, applied in the field of antibiotics, can solve the problems of low cefotaxime sodium crystal yield, poor stability of cefotaxime acid, difficult to control crystallization process, etc., and achieves the advantages of being beneficial to solvent recovery and low cost , good color grade effect

Inactive Publication Date: 2009-07-22
FUJIAN FUKANG PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the poor stability of cefotaxime acid, degradation reactions may occur at the three parts of its phthalimide side chain, β-lactam ring and acetic acid group, so thioxamic acid that has been placed for a long time will degrade to varying degrees , resulting in deeper color and lower content. Generally, thioxamic acid is recrystallized, and then sodium-transformed crystallization is performed. The existing sodium-transferred crystallization technology is mostly used in a small amount of water and organic solvents. After the cefotaxime acid and alkali react, dropwise Solvent, to sep

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] 1) In a 500ml three-necked bottle, add 14.5ml of water, 60ml of acetone, 4g of anhydrous sodium acetate, and cool down to 10°C;

[0045] 2) Add 20 g of cefotaxime acid to the mixed solution in step 1), and stir until it dissolves;

[0046] 3) After clarification, add 0.30g of activated carbon and stir at 10°C for 20 minutes;

[0047] 4) filter and wash with 15ml of 80% acetone;

[0048] 5) Combine the filtrates, control the temperature to 18°C, add 70ml of acetone dropwise, add the seed crystals, grow the crystals and stir for 0.5 hours;

[0049] 6) Slowly add 240ml of acetone dropwise;

[0050] 7) Cool down to 5°C and grow the crystal for more than 30 minutes;

[0051] 8) filter, soak and wash twice with 100ml acetone,

[0052] 9) Vacuum drying to obtain cefotaxime acid transsodium salt crystals.

[0053] The amount of seed crystals added in the above step 5) is 0.03% relative to the weight of the input cefotaxime acid; the seed crystal size is selected to be 80 m...

Embodiment 2

[0058] 1) In a 500ml three-necked bottle, add 14.5ml of water, 60ml of acetone, 4g of anhydrous sodium acetate, and cool down to 15°C;

[0059] 2) Add 20 g of cefotaxime acid to the mixed solution in step 1), and stir until it dissolves;

[0060] 3) After clarification, add 0.30g of activated carbon and stir at 15°C for 20 minutes;

[0061] 4) filter and wash with 15ml of 80% acetone;

[0062] 5) Combine the filtrates, control the temperature to 20°C, add 70ml of acetone dropwise, add the seed crystals, grow the crystals and stir for 2 hours;

[0063] 6) Slowly add 300ml of acetone dropwise;

[0064] 7) Cool down to 10°C and grow the crystal for more than 30 minutes;

[0065] 8) filter, soak and wash twice with 100ml acetone,

[0066] 9) Vacuum drying to obtain cefotaxime acid transsodium salt crystals.

[0067] The amount of seed crystals added in step 5) above is 0.1% of the weight of the input cefotaxime acid; the size of the seed crystals is selected to be 120 mesh. ...

Embodiment 3

[0072] 1) In a 500ml three-necked bottle, add 14.5ml of water, 60ml of acetone, 4g of anhydrous sodium acetate, and cool down to 12°C;

[0073] 2) Add 20 g of cefotaxime acid to the mixed solution in step 1), and stir until it dissolves;

[0074] 3) After clarification, add 0.30g of activated carbon and stir at 12°C for 20 minutes;

[0075] 4) filter and wash with 15ml of 80% acetone;

[0076] 5) Combine the filtrates, control the temperature to 19°C, add 70ml of acetone dropwise, add the seed crystals, grow the crystals and stir for 1 hour;

[0077] 6) Slowly add 270ml of acetone dropwise;

[0078] 7) Lower the temperature to 8°C and grow the crystal for more than 30 minutes;

[0079] 8) filter, soak and wash twice with 100ml acetone,

[0080] 9) Vacuum drying to obtain cefotaxime acid transsodium salt crystals.

[0081] The amount of seed crystals added in the above step 5) is 0.05%-0.8% relative to the weight of the input cefotaxime acid; the seed crystal size is selec...

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PUM

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Abstract

The invention provides a crystallization method for concerting cefotaxime acid to sodium salt; the method comprises the steps: water, acetone and anhydrous sodium acetate are added into a three-necked bottle; cefotaxime acid is added into the three-necked bottle after the temperature is lowered; then, the mixture in the three-necked bottle is stirred to cause the mixture to dissolve; next, added with active carbon, stirred, filtered and washed with acetone; the filter liquor is combined, added with acetone by dripping and added with crystal seeds, crystallized, stirred, added with acetone by dripping again, cooled, crystallized, filtered, soaked and washed with acetone for twice and dried in vacuum to obtain cefotaxime sodium crystal. The crystallization method has the advantages of simple menstruum, simplicity and feasibility, low cost, good crystal forms, good mobility, easy sub-package, high clarity and good color grade, thus being suitable for large-scale promotion and application and having obvious economic benefits.

Description

technical field [0001] The invention belongs to the technical field of antibiotics, and more specifically relates to a method for crystallizing cefotaxime acid into sodium salt. Background technique [0002] Cefotaxime sodium (cefotaxime sodium) (I) is a third-generation cephalosporin, which has a wide antibacterial spectrum, stable and safe characteristics, because it has an aminothiazolyl-cis-methoxyiminoacetyl group to bind the cephalosporin skeleton The aminoacylated structure at the seventh position in the drug has antibacterial activity against G(-) bacillus and drug-resistant bacteria that is dozens or hundreds of times stronger than that of the first and second-generation cephalosporins, and has the characteristics of less nephrotoxicity. The price is relatively cheap, so it is the most widely used antibiotic variety in clinical practice. However, due to the poor stability of cefotaxime acid, degradation reactions may occur at the three parts of its phthalimide side...

Claims

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Application Information

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IPC IPC(8): C07D501/34C07D501/04C07D501/12
Inventor 蔡彬姚志扬
Owner FUJIAN FUKANG PHARMA
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