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A kind of preparation method of deacetylceftiamidine

A technology of acetylceftiamidine and cefathiamidine, which is applied in the field of medicine, can solve problems such as inability to confirm the structure, and achieve the effects of low cost, simple operation and high purity

Active Publication Date: 2018-02-23
GUANGZHOU BAIYUSN TIANXIN PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The LC-MS method reported in the literature can only analyze and deduce the structure of deacetylceftiamidine based on the result information, and the structure cannot be confirmed because no sample is prepared.

Method used

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  • A kind of preparation method of deacetylceftiamidine
  • A kind of preparation method of deacetylceftiamidine
  • A kind of preparation method of deacetylceftiamidine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Add 20g of cefathiamidine, add 50ml of purified water, control the temperature at 20°C to 25°C, stir until it dissolves, add 1.6g of immobilized acetylesterase, and continuously and slowly add triethylamine to control the pH to 7.0 to 9.0, and stir to react until The pH remained essentially unchanged. Filter to remove the enzyme, add hydrochloric acid dropwise to adjust the pH to 5.0-5.5, concentrate the filtrate to dryness under reduced pressure, wash with dichloromethane, filter, and dry in vacuo to obtain deacetylceftiamidine.

[0026] The purity was 98% as detected by HPLC.

Embodiment 2

[0028] Add 20g of cefathiamidine, 60ml of purified water and 3ml of methanol, control the temperature at 20°C-25°C, stir until it dissolves, add 2.0g of immobilized acetylesterase, and continuously and slowly add ammonia water dropwise to control the pH 7.0-9.0, and stir to react until the pH remained basically unchanged. Filter to remove the enzyme, add hydrochloric acid dropwise to adjust the pH to 5.0-5.5, concentrate the filtrate to dryness under reduced pressure, wash with acetone, filter, and vacuum-dry to obtain deacetylceftiamidine.

[0029] The purity was 97% as detected by HPLC.

Embodiment 3

[0031] Add 20g of cefathiamidine, 70ml of purified water and 7ml of ethanol, control the temperature at 20°C-25°C, stir until it dissolves, add 2.2g of immobilized acetylesterase, and continuously and slowly drop triethylamine to control the pH 7.0-9.0, The reaction was stirred until the pH remained essentially constant. Filter to remove the enzyme, add hydrochloric acid dropwise to adjust the pH to 5.0-5.5, concentrate the filtrate to dryness under reduced pressure, wash with dichloromethane, filter, and dry in vacuo to obtain deacetylceftiamidine.

[0032] The purity was 97% as detected by HPLC.

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Abstract

The invention relates to a preparation method of deacetylceftiamidine, which is suitable for pharmaceutical enterprises, and discloses step (1): dissolving cefathiamidine in water or water containing 5% to 20% organic solvent, and controlling the temperature to 20°C ~35°C, add 0.8~1.2 times of immobilized acetyl esterase, add pH regulator to control system pH7.0~9.0 at the same time, stir and react; the amount of water or water containing organic solvent is 2.5~ 4.0 times; step (2): after the reaction, filter, adjust the pH to 5.0-5.5, concentrate under reduced pressure, wash, filter, and vacuum-dry to obtain deacetylceftiamidine as a solid. The invention adopts an enzymatic method to prepare deacetylceftiamidine with a high purity of not less than 97%, and can be used as a reference substance for the quality control of cefathiamidine bulk drug and its preparation.

Description

technical field [0001] The invention belongs to the technical field of medicine, and relates to a preparation method of deacetylceftiamidine. technical background [0002] The adverse reactions of drugs in clinical use are not only related to the pharmacological activity of the drug itself, but also closely related to the impurities in the drug. Therefore, impurity research is the focus of drug quality research, quality control and safety research, involving qualitative research and quantitative research. Research runs through the whole process of pharmaceutical research. [0003] Impurity reference substances are an important key to drug impurity research, but the impurities of most drugs are not provided with reference substances, that is, the acquisition of impurity reference substances has become the bottleneck of most drug impurity studies. [0004] The sources of impurities include process impurities (incompletely reacted reactants and reagents, intermediates, by-prod...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C12P35/00
Inventor 谭胜连司徒小燕文青闵翠娥陆媛郭泽彬贾永兵
Owner GUANGZHOU BAIYUSN TIANXIN PHARMA
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