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Preparation process for cefuroxime acid crystallization

A technology for cefuroxime acid and a preparation process, which is applied to the field of preparation technology of cefuroxime acid crystallization, can solve the problems of filtration, difficulty in drying, long production cycle, small product particle size, etc. Complete, lower production cost effect

Inactive Publication Date: 2017-03-08
HEBEI UNIVERSITY OF SCIENCE AND TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] At present, in the production process of this product, there are generally problems such as small particle size, high viscosity of crystal slurry, difficulty in filtration and drying, etc., resulting in long production cycle and high production cost.

Method used

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  • Preparation process for cefuroxime acid crystallization

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Take 360mL of the cefuroxime acid feed solution prepared by the upstream process and add it to a 500mL crystallizer, control the temperature at 22°C, and stir at a rate of 100r / min to obtain Liquid A. Add 10.8mL of dichloromethane and 7.2mL of acetonitrile to Liquid A, Get Liquid B. Add hydrochloric acid dropwise to liquid B until the pH value is 3.9. During this process, the stirring speed is 180r / min, so that hydrochloric acid and liquid B can be mixed rapidly to obtain liquid C. Add seed crystals to liquid C, the amount of seed crystals is 0.7g, and grow crystals. During crystal growth, the stirring speed is kept at 110r / min, and the crystal growth time is 20min, to obtain crystal slurry A. Continue to add hydrochloric acid dropwise to the magma A, stop adding acid when the pH value is adjusted to 2.0, the acid dripping time is 4.5h, and the stirring speed is 100r / min to obtain the magma B. Crystal slurry B was grown for 15 minutes at a stirring speed of 110 r / min t...

Embodiment 2

[0035] Take 200mL of the cefuroxime acid feed liquid prepared in the upstream process and add it to a 500mL crystallizer, control the temperature at 24°C, and stir at a rate of 105r / min to obtain Liquid A, and add 6mL of tetrahydrofuran to Liquid A to obtain Liquid B. Add hydrochloric acid dropwise to liquid B until the pH value is 4.2. During this process, the stirring speed is 180r / min, so that hydrochloric acid and liquid B can be mixed rapidly to obtain liquid C. Add seed crystals to liquid C, the amount of seed crystals is 0.7g, and grow crystals. During crystal growth, the stirring speed is kept at 120r / min, and the crystal growth time is 35min, to obtain crystal slurry A. Continue to add hydrochloric acid dropwise to the magma A, stop adding acid when the pH value is adjusted to 1.3, the acid dripping time is 4 hours, the stirring speed is 130r / min, and the magma B is obtained. The crystal slurry B was grown for 25 minutes, and the stirring speed was 120 r / min during th...

Embodiment 3

[0037] Take 200mL of the cefuroxime acid feed solution prepared by the upstream process and add it to a 500mL crystallizer, control the temperature at 22°C, and stir at a rate of 100r / min to obtain Liquid A. Add 10mL of isopropanol and 4mL of acetonitrile to Liquid A to obtain liquid b. Add hydrochloric acid dropwise to liquid B until the pH value is 4.1. During this process, the stirring speed is 200r / min, so that hydrochloric acid and liquid B can be mixed rapidly to obtain liquid C. Add seed crystals to liquid C, the amount of seed crystals is 0.3g, and grow crystals. During the crystal growth, the stirring speed is kept at 110r / min, and the crystal growth time is 40min, to obtain crystal slurry A. Continue to add hydrochloric acid dropwise to magma A, and stop adding acid when the pH value is adjusted to 2.5. The acid dripping time is 7 hours, and the stirring speed is 150r / min to obtain magma B. Crystal slurry B was grown for 15 minutes at a stirring speed of 100 r / min t...

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Abstract

The invention belongs to the technical field of crystallization of pharmaceutical intermediates, and discloses a preparation process for cefuroxime acid crystallization. The process provided by the invention comprises the following concrete steps: adding a cefuroxime acid material liquid prepared in an upstream process into a crystallizer, adding a proper amount of a crystal modifier, adjusting a certain temperature and stirring rate; dropwise adding hydrochloric acid and adjusting the pH value of the mixed solution to a certain value, adding a proper amount of seed crystals, and allowing crystals to grow; adjusting the stirring rate and the hydrochloric acid dropwise adding rate, continuously dropwise adding the hydrochloric acid, and after the completion of dropwise adding, allowing the crystals to grow again; and carrying out filtering, washing and vacuum drying so as to obtain a cefuroxime acid crystallization product. The cefuroxime acid crystal obtained by using the crystallization process provided by the invention has high purity, complete crystal habits and proper particle sizes and particle-size distribution, solves common problems like small product particle size, large crystal slurry viscosity, difficult filtration and drying in the production process of cefuroxime acid in the prior art, shortens the production cycle of products, and reduces production cost.

Description

technical field [0001] The invention belongs to the technical field of pharmaceutical intermediate crystallization, and in particular relates to a preparation process of cefuroxime acid crystallization. Background technique [0002] Cefuroxime Acid, English name Cefuroxime Acid, also known as Cefuroxime; Cefuroxime; Fuximemycin. Its chemical name is: (6R,7R)-7-[2-furyl(methoxyimino)acetamido]-3-carbamoyloxymethyl-8-oxo-5-thia-1-nitrogen Heterobicyclo[4.2.0]oct-2-ene-2-carboxylic acid, relative molecular weight: 424.39, molecular formula: C 16 h 16 N 4 o 8 S. The chemical structural formula is as follows: [0003] [0004] Cefuroxime belongs to the second-generation cephalosporin antibiotics. It is characterized by broad antibacterial spectrum, low renal toxicity and strong permeability. The drug is relatively stable to β-lactamase. Many β-lactamase-producing bacteria include german Both Lambert-positive and negative bacteria are sensitive to it, and its effect is e...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D501/34C07D501/12
CPCC07D501/34C07D501/12
Inventor 刘宝树孙华种悦晖宋梦燕
Owner HEBEI UNIVERSITY OF SCIENCE AND TECHNOLOGY
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