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Preparation method of cefotaxime acid

A technology of cefotaxime acid and cefotaxime sodium, which is applied in the field of medicine, can solve the problems that cefotaxime acid cannot meet the production demand and affect the quality of cefotaxime sodium, and achieve a product with good quality, easy implementation and simple operation process Effect

Active Publication Date: 2022-04-15
NORTH CHINA PHARMA HEBEI HUAMIN PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In the actual production of thioxime sodium, due to the influence of technology or production conditions (such as storage, transportation process, etc.), there will be unqualified products of related substances or content detection items, and the cefotaxime acid recovered by the prior art cannot meet the production demand. Affect the quality of cefotaxime sodium in subsequent production

Method used

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  • Preparation method of cefotaxime acid
  • Preparation method of cefotaxime acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Take 40g of cefotaxime sodium, add 240mL of purified water and 200mL of acetone, stir until dissolved; control the temperature at 5°C, add 0.2g of sodium metabisulfite, adjust the pH to 4.5 with citric acid-disodium hydrogen phosphate mixture; add activated carbon and stir 30min. Filter and wash the carbon cake with 5 mL of purified water.

[0032] Combine the filtrate and lotion, add glacial acetic acid dropwise under the condition of temperature control at 10°C to adjust the pH of the system to 2.9, add 0.04 g of seed crystals and stir for 30 minutes to grow the crystals. Add glacial acetic acid to adjust the pH of the system to 2.9. At the same time, add 240mL of purified water. After 30 minutes, the temperature is lowered to 0°C and the crystal growth is continued for 30 minutes.

[0033] Filter, wash with 100 mL of acetone, and suck dry; dry at 35° C., and dry under vacuum for 1 hour to obtain 37.12 g of a white solid.

Embodiment 2

[0035] Take 40g of cefotaxime sodium, add 280mL of purified water and 240mL of acetone, stir until dissolved; control the temperature at 10°C, add 0.4g of sodium metabisulfite, citric acid-disodium hydrogen phosphate mixture to adjust the pH to 5.0; add activated carbon and stir for 30min . Filter and wash with 5 mL of purified water.

[0036] Combine the filtrate and lotion, add phosphoric acid dropwise under temperature control at 15°C to adjust the pH of the system to 3.1, add 0.4 g of seed crystals and stir for 30 minutes to grow the crystals. Add phosphoric acid to adjust the pH of the system to 3.1. At the same time, add 280 mL of purified water. After 30 minutes, cool down to 2°C and grow crystals for 60 minutes.

[0037] Filter, wash with 100 mL of acetone, and suck dry; dry at 35° C., and dry under vacuum for 1 hour to obtain 37.24 g of a white solid.

Embodiment 3

[0039] Take 40kg of cefotaxime sodium, add 260L of purified water, 220L of acetone, stir until dissolved; control the temperature at 8°C, add 0.3kg of sodium metabisulfite, citric acid-disodium hydrogen phosphate mixture to adjust the pH to 4.7; add activated carbon and stir for 30min . Filter and wash with 5L of purified water.

[0040] Combine the filtrate and lotion, add sulfuric acid dropwise under the condition of temperature control at 12°C to adjust the pH of the system to 3.0, add 0.2 kg of seed crystal and stir for 30 minutes to grow the crystal. At the same time, sulfuric acid was added to adjust the pH of the system to 3.0, and 260L of purified water was added at the same time, and the addition was completed in 30 minutes, and the temperature was lowered at 1°C to grow crystals for 45 minutes.

[0041] Filter, wash with 100L of acetone, and suck dry; dry at 35°C, and dry under vacuum for 1 hour to obtain 37.28kg of white solid.

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Abstract

The invention discloses a preparation method of cefotaxime acid, which belongs to the technical field of medicine, and comprises the following steps: by taking unqualified cefotaxime sodium as a raw material, dissolving the cefotaxime sodium, adding a protective agent and a phosphate solution, decoloring, dropwise adding an acid reagent to adjust the pH value of the feed liquid, adding a cefotaxime acid seed crystal, growing the crystal, filtering, and drying to obtain the cefotaxime acid. And after crystal growing is finished, continuously dropwise adding an acid reagent and water to adjust the pH value, cooling, growing the crystal, filtering and drying to obtain the cefotaxime acid. The cefotaxime acid prepared by the method disclosed by the invention has the advantages of energy conservation, environmental protection, recyclable solvent and simple operation, and the prepared cefotaxime acid has the advantages of good quality, high product content and low impurity content, and solves the problem that reworking is required for producing dirty powder due to unqualified products such as content, impurities and the like of cefotaxime sodium sometimes.

Description

technical field [0001] The invention belongs to the technical field of medicine, and relates to a preparation method of cefotaxime acid. Background technique [0002] Cefotaxime acid is used to synthesize cefotaxime sodium, which is a third-generation cephalosporin. A semi-synthetic oxime-type cephalosporin, this product has a strong effect on Gram-negative bacteria, especially Enterobacteriaceae. It is mainly used for respiratory system infection, urinary system infection, biliary tract and intestinal infection, skin and soft tissue infection, burn and bone and joint infection caused by sensitive bacteria. Cefotaxime acid chemical name: 3-acetoxymethyl-7-[2-(2-amino-4-thiazolyl)-2-methoxyimino]-acetamido-3-cephalosporin-4 -Carboxylic acid, structural formula is as follows: [0003] [0004] Patent (CN201610428435.5) "A Method for Purifying and Recovering Cefotaxime Acid from Cefotaxime Sodium" introduces a method for purifying and recovering cefotaxime acid from unqua...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D501/34C07D501/04C07D501/12
CPCC07D501/34C07D501/04C07D501/12
Inventor 贾全田洪年胡利敏任峰孙玉双刘树斌张建丽魏宝军贺娇
Owner NORTH CHINA PHARMA HEBEI HUAMIN PHARMA
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