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Preparation method of cefotaxime sodium crystal

A technology for cefotaxime sodium and cefotaxime acid is applied in the field of preparing cefotaxime sodium crystals, which can solve the problems of large seed crystal size, difficult to adjust crystal size, large supersaturation degree of cefotaxime sodium and the like, and achieve particle size distribution. Concentration, good fluidity, avoid gelling effect

Active Publication Date: 2013-09-04
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method uses a large seed crystal size and a small specific surface area, which cannot provide enough interfaces to promote crystal growth, primary nucleation is difficult to avoid, and gelation will inevitably occur.
And this method is 80% acetone volume fraction when preparing acetone-water mixed solvent, and acetone volume fraction surpasses 85% when adding seed crystal, and cefotaxime sodium supersaturation degree is bigger in the solution, and it will be difficult to regulate the later stage crystal particle size
[0013] Cefotaxime sodium reaction - the biggest advantage of using an aqueous solvent in the crystallization process is that it is non-toxic, easy to obtain, and low in cost, but the crystallization process using an aqueous solvent is prone to gelation, and cefotaxime sodium is easily formed during the crystallization process. Colloids, resulting in very unstable crystallization process, low yield, low purity and poor clarity of crystallized products, etc.

Method used

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  • Preparation method of cefotaxime sodium crystal
  • Preparation method of cefotaxime sodium crystal
  • Preparation method of cefotaxime sodium crystal

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] The temperature is 30°C, and 2.1 g of sodium acetate is dissolved in 30 mL of n-propanol-water mixed solvent with a volume fraction of n-propanol of 55%, to obtain a sodium acetate solution with a concentration of 0.07 g / mL; add 10 g of cefotaxime acid, Stir to react the cefotaxime acid in the solution to obtain a cefotaxime sodium solution; add 0.4 g of cefotaxime sodium seed crystals with a main particle size of 10 μm to the solution; add 240 mL of acetone, and the feeding time is 5 hours. After the feeding was completed, the temperature was lowered to 2°C. After the crystalline slurry was filtered, washed, and dried at 40° C. and a vacuum degree of 0.09 MPa for 20 hours, 9.29 g of cefotaxime sodium crystals were obtained.

[0031] The main particle size of the product is 12.2 μm, the product molar yield is 88.6%, and the product purity is 95.6%. The particle size distribution of the product is shown in figure 2 .

Embodiment 2

[0033] Temperature is 10 ℃, and 2.3g sodium acetate is dissolved in the ethanol-water mixed solvent 40mL that ethanol volume fraction is 70%, obtains the sodium acetate solution that concentration is 0.0575g / mL; Add cefotaxime acid 10g, stir to make cefotaxime The xamic acid was reacted in the solution to obtain a cefotaxime sodium solution; 5 mL of ethanol was added to the solution, and then 0.1 g of cefotaxime sodium seed crystals with a main particle size of 1 μm were added, and 400 mL of ethanol was added continuously for 3 hours. After feeding, the temperature was lowered to 0°C, and the crystal was grown for 2 hours. The crystal slurry was filtered, washed, and dried for 24 hours at 30° C. under a vacuum of 0.095 MPa to obtain 9.29 g of cefotaxime sodium crystals.

[0034] The main particle size of the product is 41.4μm, the molar yield of the product is 88.6%, and the product purity is 95.8%. For the particle size distribution of the product, see image 3 . The partic...

Embodiment 3

[0036]Temperature is 40 ℃, and 1.8g sodium acetate is dissolved in the methanol-water mixed solvent 30mL that methanol volume fraction is 50%, obtains the sodium acetate solution that concentration is 0.06g / mL; Add cefotaxime acid 10g, stir to make cefotaxime The xamic acid reacts in the solution to obtain a cefotaxime sodium solution; add 9 mL of acetone to the solution, then add 0.5 g of cefotaxime sodium seed crystals with a main particle size of 10 μm, and grow the crystals for 0.5 h; continue to add 270 mL of acetone, and the feeding time 8h. After feeding, the temperature was lowered to -5°C, and the crystal was grown for 1 hour. The crystal slurry was filtered, washed, and dried for 18 hours at 40° C. under a vacuum of 0.09 MPa to obtain 9.40 g of cefotaxime sodium crystals.

[0037] The main particle size of the product is 6.1 μm, the product molar yield is 89.7%, and the product purity is 95.6%.

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Abstract

The invention relates to a preparation method of a cefotaxime sodium crystal. The preparation method comprises the following steps of: dissolving sodium acetate in a mixed solvent of organic solvent and water below 10-40 DEG C, wherein the volume fraction of organic solvent in the mixed solvent is 30-70%; adding cefotaxime acid, and stirring until the cefotaxime acid reacts in the solution; adding a cefotaxime sodium crystal in the solution, then adding elution agents with a feeding time of 2-8 hours, cooling to 5 DEG C below zero to 5 DEG C; and filtering, washing and drying a crystal slurry to obtain the cefotaxime sodium crystal. By the preparation method, the phenomenon of gelatinization frequently seen in the crystallization process of the cefotaxime sodium crystal is avoided, the size distribution of the products is centralized and the major particle size is adjustable from 5mu m to 60my m, the liquidity of the product is good, the process yield is higher than 87%, and the product purity is higher than 95.5%.

Description

technical field [0001] The invention belongs to the technical field of chemical engineering crystallization, in particular to a method for preparing cefotaxime sodium crystals. Background technique [0002] Cefotaxime sodium, molecular formula C 16 h 16 N 5 o 7 S 2 Na, molecular weight 477.44, chemical name (6R,7R-3-[(acetoxy)methyl]-7-[(2-amino-4-thiazolyl)-(methoxyimino)acetamide] -8-Oxo-5-thia-1-azabicyclo[4.2.0]oct-2-ene-2-carboxylic acid sodium salt, its structural formula is shown in the following structure. Cefotaxime sodium is white to slightly yellow crystals, Odorless or slightly special odor, CAS number: 64485-93-4. [0003] [0004] Cefotaxime sodium belongs to the third-generation semi-synthetic cephalosporins, which have resistance activity to both Gram-positive and Gram-negative bacteria. Cefotaxime sodium has a strong effect on bacilli, such as Escherichia coli, Enterobacter, influenza bacillus, etc., and has a good inhibitory effect on most anaerob...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D501/34C07D501/12
Inventor 鲍颖尹永恒王永莉张海涛侯宝红高振国张美景尹秋响郝红勋谢闯
Owner TIANJIN UNIV
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