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Method of preparing vancomycin through cyclopentadiene-acrolein

A technology of vancomycin and cyclopentadiene, applied in the direction of peptides, etc., can solve the problems of slow growth of vancomycin hydrochloride crystals, difficult crystallization, and difficult crystallization, and achieve simple production methods, improved effective components, Effect of appearance color change

Inactive Publication Date: 2017-03-22
江苏海阔生物医药有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among them, the crystallization process can improve the purity of vancomycin and remove some impurities such as pigments. However, due to the slow growth of vancomycin hydrochloride crystals, the crystallization process is easily disturbed by impurities, and the crystallization is difficult. Only the crude extract through ion exchange and decolorization hard to crystallize

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  • Method of preparing vancomycin through cyclopentadiene-acrolein

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preparation example Construction

[0019] see figure 1 , the invention provides a kind of preparation method that prepares vancomycin by cyclopentadiene-acrolein, comprises the following steps:

[0020] a. Mixing cyclopentadiene-acrolein and vancomycin aqueous solution to obtain a first mixture, and making the pH of the first mixture less than 6, dividing the first mixture into an oil phase and an aqueous phase, Separate the oil phase to obtain an extract containing vancomycin;

[0021] b. Precipitate the vancomycin-containing extract obtained in step a in a precipitation container to obtain a crystal slurry, and stir the crystal slurry to continuously adjust the pH value to the required level until complete precipitation to obtain a crystal precipitate ;

[0022] c. Dissolving the crystal precipitate obtained in step b into an aqueous solution, and then converting it to vancomycin through an anion exchange resin.

[0023] According to step a, the pH range of the cyclopentadiene-acrolein is 1.0-3.0.

[0024...

Embodiment 1

[0029] Include the following steps:

[0030] a. Mix cyclopentadiene-acrolein and vancomycin aqueous solution to obtain the first mixture, and make the pH value of the first mixture 6, divide the first mixture into an oil phase and an aqueous phase, separate The oil phase is removed to obtain an extract containing vancomycin, and the pH of the cyclopentadiene-acrolein is 3.0;

[0031] b. Precipitate the vancomycin-containing extract obtained in step a in a precipitation container to obtain a crystal slurry, and stir the crystal slurry to continuously adjust the pH value to the required level until complete precipitation to obtain a crystal precipitate , the initial temperature of the crystallization process is 60°C; the end temperature of the crystallization process is 30°C; the cooling rate of the crystallization process is 5°C / min;

[0032] c. Dissolving the crystal precipitate obtained in step b into an aqueous solution, and then converting it to vancomycin through an anion...

Embodiment 2

[0034] Include the following steps:

[0035] a. Mix cyclopentadiene-acrolein and vancomycin aqueous solution to obtain the first mixture, and make the pH value of the first mixture 3, divide the first mixture into an oil phase and an aqueous phase, separate The oil phase is removed to obtain an extract containing vancomycin, and the pH range of the cyclopentadiene-acrolein is 1.0;

[0036] b. Precipitate the vancomycin-containing extract obtained in step a in a precipitation container to obtain a crystal slurry, and stir the crystal slurry to continuously adjust the pH value to the required level until complete precipitation to obtain a crystal precipitate , the initial temperature of the crystallization process is 25°C; the end temperature of the crystallization process is 0°C; the cooling rate of the crystallization process is 0.5°C / min;

[0037] c. Dissolving the crystal precipitate obtained in step b into an aqueous solution, and then converting it to vancomycin through a...

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Abstract

The invention discloses a method of preparing vancomycin through cyclopentadiene-acrolein. According to the preparation method, cyclopentadiene-acrolein and a vancomycin water solution are mixed to obtain a first mixture, then the pH value of the first mixture is adjusted to be smaller than 6; the first mixture is divided into an oil phase and a water phase, and the oil phase is separated out from the first mixture so as to obtain the extract containing vancomycin. The effective component of prepared vancomycin is largely improved. Other impurities are largely reduced. The purity is very high, and the chromatographic purity can reach more than 95%. At the same time, the appearance and color of the product are prominently improved. The prepared vancomycin can be orally taken or applied to injection. The manufacturing method is simple, and the technology is suitable for massive production.

Description

technical field [0001] The invention relates to the technical field of preparation methods of vancomycin, in particular to a preparation method of vancomycin by cyclopentadiene-acrolein. Background technique [0002] Vancomycin is an antibiotic with the molecular formula C66H74Cl2N9O24. Its half-life: 4 to 8 hours, 9 days for renal failure, ineffective against anaerobic bacteria and Gram-negative bacteria, and will not be removed by hemodialysis. The "superbug" NDM-1 that appeared in India and other South Asian countries has spread to the United Kingdom, the United States, Canada, Australia, the Netherlands and other countries. Domestic experts say that the South Asian superbug will not become a pandemic, and vancomycin can be effective. [0003] Vancomycin belongs to glycopeptide macromolecular antibiotics. Vancomycin is more powerful and will be used when other antibiotics are ineffective against bacteria. It is mainly used for systemic and intestinal infections caused b...

Claims

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Application Information

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IPC IPC(8): C07K9/00C07K1/36C07K1/30C07K1/18
Inventor 苗玉武吕祖平刘永刚王丹丹刘言华
Owner 江苏海阔生物医药有限公司
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