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Method for preparing cefotaxime sodium crystal

A technology for cefotaxime sodium and crystals is applied in the field of preparation of cefotaxime sodium crystals, which can solve the problems of reducing heat transfer, mass transfer efficiency, adding a large amount of elution agent, and unavoidable gel formation, and achieves easy gelation. The effect of condensation, large crystal size and concentrated distribution

Active Publication Date: 2015-09-09
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The method disclosed in CN103319504A also needs to add seed crystals, and the amount of eluting agent added before seed crystals is too much, and gelation is still difficult to avoid
However, the co-solvent is highly irritating, inconvenient to operate, and harmful to health
[0005] The method for above-mentioned preparation cefotaxime sodium crystal all is that poor solvent is added in cefotaxime sodium solution, and this process is particularly prone to gelation phenomenon: along with poor solvent adds, supersaturation constantly increases, and cefotaxime sodium molecule It will interweave into a network structure through self-assembly and wrap the solvent, and the appearance is in a semi-fluid viscous gel state. Cefotaxime sodium is enriched in the viscous colloid and separates from the main solution
The occurrence of gelation seriously affects the product quality, and the gelatinous substance adheres to the stirring paddle or the wall of the vessel, which reduces the heat transfer and mass transfer efficiency, and even affects the entire operation process

Method used

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  • Method for preparing cefotaxime sodium crystal
  • Method for preparing cefotaxime sodium crystal
  • Method for preparing cefotaxime sodium crystal

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Prepare the formamide solution of 0.029g / mL sodium acetate, add cefotaxime acid, the mol ratio of sodium acetate and cefotaxime acid is 1.2:1, add active carbon decolorization after stirring reaction, filter to obtain clarified cefotaxime sodium solution, The concentration is 0.14g / mL. Take 30mL of cefotaxime sodium solution and add it dropwise to 300mL of methanol at 20°C within 100min. After the dropwise addition, the temperature was lowered to 5° C. at a cooling rate of 1° C. / min, filtered, washed with methanol, and dried at -70° C. under an absolute pressure of 36 Pa for 24 hours to obtain amorphous cefotaxime sodium powder with a molar yield of 97%. The obtained amorphous powder was left standing in a water atmosphere with a relative humidity of 32% at 30°C for 24h, washed and filtered, and then dried under reduced pressure at 40°C for 36h to obtain a crystalline product with a molar yield of 84%. The total yield of the process is 81.5%, and the crystal product co...

Embodiment 2

[0028]Prepare 0.13g / mL sodium acetate N-N dimethylformamide solution, add cefotaxime acid, the molar ratio of sodium acetate to cefotaxime acid is 1.1:1, add activated carbon to decolorize after stirring the reaction, filter to obtain clarified cefotaxime Sodium oxime solution, the concentration is 0.70g / mL. Take 30mL of cefotaxime sodium solution and add dropwise to 300mL of ethanol and ethyl acetate mixed solvent at 20°C within 10min. After the dropwise addition, the temperature was lowered to 5°C at a cooling rate of 1°C / min, filtered and washed with ethyl acetate. Dry at -60° C. for 12 hours under an absolute pressure of 100 Pa to obtain amorphous cefotaxime sodium powder with a molar yield of 96%. The obtained amorphous powder was left standing in 2° C. saturated water vapor for 48 hours, washed and filtered, and then dried under reduced pressure at 40° C. for 28 hours to obtain a crystalline product with a molar yield of 83.6%. The total molar yield of the process is 8...

Embodiment 3

[0031] Prepare the aqueous solution of sodium acetate of 0.048g / mL, add cefotaxime acid, the mol ratio of sodium acetate and cefotaxime acid is 1:1, add activated carbon decolorization after stirring reaction, filter and obtain clear cefotaxime sodium solution, concentration 0.28g / mL. Take 30 mL of cefotaxime sodium solution and add dropwise to 150 mL of ethyl acetate at 10°C within 20 min. After the dropwise addition, the temperature was lowered to 0°C at a cooling rate of 0.2°C / min, filtered, washed with ethyl acetate, and dried at -60°C under an absolute pressure of 100 Pa for 36 hours to obtain the amorphous powder of cefotaxime sodium. The molar yield was 98%. The obtained amorphous powder was left standing in saturated water vapor at 20°C for 24h, washed and filtered, and then dried under reduced pressure at 40°C for 24h to obtain a crystalline product with a molar yield of 85.5%. The total molar yield of the process is 83.8%, and the crystal product content is 95.8%. ...

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Abstract

The invention discloses a novel method for preparing a cefotaxime sodium crystal. The method comprises the following steps: adding a cefotaxime sodium solution into an organic solvent the volume of which is 5-15 times that of the cefotaxime sodium solution at 10-30 DEG C, cooling to 0-9 DEG C, filtering, washing and drying to cefotaxime sodium amorphous-form powder; and at 2-40 DEG C, putting the amorphous-form powder into an organic solvent atmosphere or into a water atmosphere with relative humidity of 32-100%, standing and transferring the crystal for 24-48 hours, and washing, filtering and drying to obtain a cefotaxime sodium crystal product. According to the method, a jelling problem in a dissolving-out process is effectively avoided, the operation is simple, and the total molar yield in the process is higher than 80%. The crystal product has a main grain size which can reach 100 microns, is high in content, high in degree of crystallinity and good in stability.

Description

technical field [0001] The invention belongs to the technical field of chemical engineering medicine crystallization, and in particular relates to a preparation method of cefotaxime sodium crystal. Background technique [0002] Cefotaxime sodium (cefotaxime sodium) is a third-generation semi-synthetic cephalosporin, which has the advantages of broad antibacterial spectrum, strong antibacterial effect, and small toxic and side effects. It is clinically used in the treatment of various sensitive bacterial infections. Cefotaxime sodium molecular formula C 16 h 16 N 5 o 7 S 2 Na, molecular weight 477.44, chemical name is (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 below. [0003] [0004] The preparation process of cefotaxime sodium crystals currently reported is generally divided into two steps: firstly, the cefotaxime sodium soluti...

Claims

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Application Information

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IPC IPC(8): C07D501/34C07D501/12
CPCC07D501/12C07D501/34
Inventor 鲍颖高振国侯宝红郝红勋王召尹秋响王静康
Owner TIANJIN UNIV
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