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A kind of preparation method of cefathiamidine

A technology of cefathiamidine and cefathiamidine, which is applied in the field of medicine, can solve the problems that there are no literature and patent reports on the preparation method of cefathiamidine and its structural confirmation, and achieve low cost, mild conditions and high purity Effect

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

[0009] After review, there are no literature and patent reports on the preparation method of cefathiamidine and its structural confirmation

Method used

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  • A kind of preparation method of cefathiamidine
  • A kind of preparation method of cefathiamidine
  • A kind of preparation method of cefathiamidine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Add 20 g of cefathiamidine to 50 ml of water, control the temperature at 20°C to 25°C, and stir until dissolved. 1.6 g of immobilized acetylesterase was added, and triethylamine was continuously added dropwise to control the pH to 7.0-9.0 until it remained basically unchanged. Filter to remove enzymes, add 50ml of water, add concentrated hydrochloric acid dropwise to adjust pH<1, and stir for 3 hours. Filter, wash with water, and dry in vacuum to obtain cefathiamidine.

[0026] The purity was 96% 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 enzymes, add 140ml of water to the filtrate, add dilute sulfuric acid dropwise to adjust pH<1, and stir for 6 hours. Filter, wash with water, and dry in vacuum to obtain cefathiamidine.

[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 25°C to 30°C, stir until it dissolves, add 2.2g of immobilized acetylesterase, and continuously and slowly drop triethylamine to control the pH to 7.0 to 9.0, The reaction was stirred until the pH remained essentially constant. Filter to remove enzymes, add 255ml of water to the filtrate, add hydrobromic acid dropwise to adjust pH<1, and stir for 9 hours. Filter, wash with water, and dry in vacuum to obtain cefathiamidine.

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

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Abstract

The invention discloses a preparation method of cefathiamidine lactone. The preparation method comprises the following steps: dissolving cefathiamidine into water or water containing 5 to 20 percent of an organic solvent, controlling the temperature to be 20 to 35 DEG C, adding 0.8 to 1.2 times of immobilized acetylase, adding a pH modifier to control system pH value to be 7.0 to 9.0, and stirring for reaction; after the reaction, filtering to remove enzyme and adding water for dilution, adding acid until the pH value is lower than 1.0, dissolving out solids, filtering, washing and drying until obtaining the cefathiamidine lactone. The yield of the water or the water containing the organic solvent is 2.5 to 4.0 times of that of cefathiamidine. The method provided by the invention adopts enzymatic reaction, the operation is simple, the prepared cefathiamidine lactone is high in purity and can be used for quality control to crude drug and the preparations of the cefathiamidine lactone.

Description

technical field [0001] The invention belongs to the technical field of medicine, and relates to a preparation method of cefathiamidine. 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-products, ...

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