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Cefixime side chain acid crystal form and preparation method thereof

A technology of cefixime side chain acid and crystal form, which is applied in the field of cefixime side chain acid crystal form and its preparation, can solve problems such as poor stability of cefixime side chain acid, achieve uniform primary particle size distribution, and process operation Simple and stable effect

Pending Publication Date: 2022-04-12
SHANDONG JINCHENG KERUI CHEMICAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The cefixime side chain acid stability synthesized by the prior art is poor

Method used

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  • Cefixime side chain acid crystal form and preparation method thereof
  • Cefixime side chain acid crystal form and preparation method thereof
  • Cefixime side chain acid crystal form and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Dissolve 16g of cefixime side-chain acid in 800ml of 20wt.% methanol aqueous solution in a 1000ml silk bottle; ultrasonically treat for 80min at 40°C with an ultrasonic frequency of 60KHz, filter after dissolving; put the resulting filtrate into a jacket The temperature in the kettle was slowly lowered to -8°C in 120 minutes, the pressure in the jacketed kettle was -0.03MPa, and the crystallization was carried out at a stirring speed of 40r / min. After the crystals were precipitated, the crystallization was carried out for 120 minutes; when the system was obviously turbid, the stirring Slowly increase the speed to 150r / min, maintain the temperature at -8~-10°C, and continue to grow the crystal for 150min; filter and wash the filter cake with a solvent of 20wt.% methanol aqueous solution; then put the filter cake at a temperature of 40°C and a vacuum of 0.1MPa Under vacuum drying 120min, obtain white granular cefixime side-chain acid crystal 14.06g, yield is 87.87%, and HP...

Embodiment 2

[0031] Dissolve 13g of cefixime side-chain acid in 800ml of 40wt.% methanol aqueous solution in a 1000ml silk bottle, ultrasonically treat for 90min at 39°C, the ultrasonic frequency is 90KHz, filter after dissolving; put the gained filtrate into the jacket Slowly lower the temperature in the kettle to -7°C in 130min, the pressure in the jacketed kettle is -0.04MPa, and crystallize at a stirring speed of 50r / min. After the crystals are precipitated, crystallize for 120min; when the system is obviously turbid, stir Slowly increase the speed to 130r / min, maintain the temperature at -8~-10°C, and continue to grow the crystal for 180min; filter and wash the filter cake with a solvent of 40wt.% methanol aqueous solution; then put the filter cake at a temperature of 40°C and a vacuum of 0.08MPa Drying under vacuum for 120 min gave 11.08 g of white granular cefixime side-chain acid crystals with a yield of 85.23% and an HPLC purity of 99.85%, which was detected as crystal form B by X-...

Embodiment 3

[0033] Dissolve 15g of cefixime side-chain acid in 800ml of 60wt.% methanol aqueous solution in a 1000ml silk bottle, ultrasonically treat for 150min at 40°C, the ultrasonic frequency is 80KHz, filter after dissolving; put the obtained filtrate into the jacket The temperature in the kettle was slowly lowered to -10°C in 150 minutes, the pressure in the jacketed kettle was -0.03MPa, and the crystallization was carried out at a stirring speed of 50r / min. After the crystals were precipitated, the crystallization was carried out for 150 minutes; Slowly increase the speed to 150r / min, maintain the temperature at -8~-10°C, and continue to grow the crystal for 180min; filter and wash the filter cake with a solvent of 60wt.% methanol aqueous solution; then put the filter cake at a temperature of 40°C and a vacuum of 0.09MPa Dry under vacuum for 90 minutes to obtain 12.97 g of white granular cefixime side-chain acid crystals with a yield of 86.47% and an HPLC purity of 99.87%, which was...

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Abstract

The invention belongs to the technical field of medicine crystallization, and particularly relates to a cefixime side chain acid crystal form and a preparation method thereof. The method comprises the following steps: dissolving cefixime side chain acid in a methanol aqueous solution, ultrasonically dissolving, and filtering; cooling the obtained filtrate in a jacketed kettle, crystallizing and growing the crystal while stirring, increasing the stirring speed to continue growing the crystal, and filtering; and washing and drying the obtained filter cake to obtain the cefixime side chain acid crystal form B. The HPLC (high performance liquid chromatography) content of the crystal form B of the side chain acid of the sporicloxime reaches 99.80% or above, and the crystal form B can be stored at room temperature for 6 months, has good stability and is very beneficial to storage of medicines; no aggregation phenomenon exists among crystals, and the main particle size distribution is uniform; according to the preparation method of the crystal form B of the cefixime side chain acid, the single-pass molar yield in the crystallization process is 85% or above, the technological operation is simple, and the preparation method is suitable for industrial production.

Description

technical field [0001] The invention belongs to the technical field of drug crystallization, and in particular relates to a cefixime side-chain acid crystal form and a preparation method thereof. Background technique [0002] Cefixime side chain acid, also known as thioesteroxamic acid, the English name is (Z)-2-(tert-MethoxycarbonylMethoxyimino)-2-(2-Aminothiazol-4-yl)Acetic Acid, the chemical name is (Z)- 2-(2-aminothiazol-4-yl)-2-(methoxycarbonylmethoxy-imino)acetic acid, the chemical formula is C 8 h 9 N 3 o 5 S. [0003] Cefixime is the third generation of oral cephalosporin antibiotics. It is an oral broad-spectrum cephalosporin. Studies in vivo and in vitro have shown that the drug has a broad antibacterial spectrum and is effective against Streptococcus pyogenes, Pneumococcus, Streptococcus agalactiae, Neisseria gonorrhoeae, influenza Most Enterobacteriaceae bacteria such as Bacillus, Morakata, Escherichia coli, and Klebsiella pneumoniae have good antibacterial ...

Claims

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Application Information

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IPC IPC(8): C07D277/593
Inventor 王辉刘镇刘艳春房硕司维森
Owner SHANDONG JINCHENG KERUI CHEMICAL CO LTD
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