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Low crystal-water ceftriaxone crystals and preparation method thereof

A technology of ceftriaxone sodium and low crystallization, which is applied in the field of ceftriaxone sodium crystals and its preparation, and can solve problems affecting the quality of ceftriaxone and affecting the safety and effectiveness of ceftriaxone

Inactive Publication Date: 2010-06-23
XIANGBEI WELMAN PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The existence of crystal water has an important influence on the stability of ceftriaxone sodium product, and ceftriaxone sodium crystals containing 3.5 crystal water make ceftriaxone sodium prone to degradation reaction during storage, produce degradation products, and affect ceftriaxone sodium. The quality of pine, ultimately affecting the safety and effectiveness of ceftriaxone
Therefore, removing or reducing the water of crystallization in ceftriaxone sodium crystals is of great significance for the stability of the product and the final clinical efficacy, but there is no relevant patent or literature report at present

Method used

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  • Low crystal-water ceftriaxone crystals and preparation method thereof
  • Low crystal-water ceftriaxone crystals and preparation method thereof
  • Low crystal-water ceftriaxone crystals and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Embodiment 1: One molecule contains the preparation method of 2.5 crystal water ceftriaxone sodium crystals

[0027] Add 160 mL of solvent water-absolute ethanol solution (volume ratio 1:3) into a jacketed crystallizer, add 45 g of ceftriaxone sodium salt, control the crystallization temperature at 15 ° C, add dropwise 300 mL of absolute ethanol, and add crystallization Seed or 0.2g, after growing the crystal for 20min, continue to add 400mL of absolute ethanol dropwise. Vacuum filter and wash twice with 300 mL of absolute ethanol. Dry under vacuum at 40° C. for 2 hours. Get 4 g of obtained ceftriaxone sodium crude crystals, add 4 g of absolute ethanol, and reflux for 4.5 hours. Dry under vacuum at 60°C for 2.5 hours to obtain ceftriaxone sodium crystals containing 2.5 crystal waters per molecule.

[0028] Wherein: ethanol can replace with formic acid, acetic acid, methyl alcohol, ethanol, n-propanol, isopropanol, n-butanol or isobutanol.

[0029] Among them: the dr...

Embodiment 2

[0030] Embodiment 2: One molecule contains the preparation method of 2.5 crystal water ceftriaxone sodium crystals

[0031] Add solvent water-acetone solution (volume ratio is 1:4) 120ml in the crystallizer with jacket, add 45g ceftriaxone sodium salt, control crystallization temperature to be 80 ℃, add dropwise absolute ethanol 300mL, add crystal seed or 0.2g, after growing the crystal for 20min, continue to add 400mL of formic acid dropwise. Vacuum filter and wash twice with 300 mL of acetone. Dry under vacuum at 100°C for 0.5 hours. Get 4 g of obtained ceftriaxone sodium crude crystals, add 20 g of n-butanol, and reflux for 0.5 hour. Dry under vacuum at 40°C for 0.5 hour to obtain ceftriaxone sodium crystals containing 2.5 crystal waters per molecule.

[0032] Among them: the drying temperature and time of the last step can be changed within a certain range, and the drying time can be shortened by about 0.5 hours for every 10°C increase in temperature.

Embodiment 3

[0033] Embodiment 3: One molecule contains the preparation method of 2.0 crystal water ceftriaxone sodium crystals

[0034] Add 160 mL of solvent water-chloroform solution (volume ratio 1:3) into a jacketed crystallizer, add 45 g of ceftriaxone sodium salt, control the crystallization temperature at 5 ° C, add dropwise 300 mL of absolute ethanol, and add crystal Seed or 0.2g, after growing the crystal for 20min, continue to add 400mL of the mixture of ethanol and isopropanol dropwise. Vacuum filter and wash twice with 300 mL acetic acid. Dry under vacuum at 10°C for 6 hours. Get 4 g of obtained ceftriaxone sodium crude crystals, add 4 g of n-butanol, and reflux for 5.5 hours. Drying under vacuum at 120° C. for 2 hours gave ceftriaxone sodium crystals containing 2.0 crystal water in one molecule.

[0035] Among them: the drying temperature and time of the last step can be changed within a certain range, and the drying time can be shortened by about 0.5 hours for every 10°C i...

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Abstract

The invention relates to the field of chemosynthesis, particularly discloses low crystal-water ceftriaxone crystals containing 1.5-2.5 water molecules. The invention also provides a preparation method of the low crystal-water ceftriaxone crystals. Compared with the ceftriaxone crystals in the prior art, the low crystal-water ceftriaxone crystals have better stability and wide clinical application prospect at the same time of remaining the same dynamics characteristics and antibiosis activities.

Description

technical field [0001] The invention relates to the field of chemical synthesis, in particular to ceftriaxone sodium crystals with low crystal water and a preparation method thereof. Background technique [0002] Ceftriaxone sodium (ceftriaxone sodium), also known as ceftriaxone, ceftriaxone, Junbizhi, cephalosporin, etc., chemical name: (6R, 7R)-7-[[(2-amino-4 -thiazolyl)(methoxyimino)acetyl]amino]-8-oxo-3-[[(1,2,5,6-tetrahydro-2-methyl-5,6-dioxo-1 , 2,4-triazin-3-yl)thio]methyl]-5-thio-1-azabicyclo[4.2.0]oct-2-ene-2-carboxylic acid disodium salt triple half Hydrate. Ceftriaxone sodium is a semi-synthetic long-acting, broad-spectrum third-generation cephalosporin with a mechanism of action similar to that of penicillin. It is white or off-white crystalline powder, odorless and tasteless, hygroscopic, easily soluble in water, slightly soluble in methanol, almost insoluble in chloroform or ether, and the aqueous solution is yellow to amber due to different concentrations. ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D501/36C07D501/12
Inventor 孙明杰王霆李苌清邓桂兴董卫星
Owner XIANGBEI WELMAN PHARMA CO LTD
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