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Purification method of micafungin precursor fr901379

A technology of micafungin and purification methods, which is applied in the fields of peptide preparation methods, chemical instruments and methods, organic chemistry, etc., and can solve the problems of high cost and difficult purification of micafungin

Active Publication Date: 2019-12-03
CHENGDU YATU BIOLOGICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] One of the purposes of the present invention is to provide a method for crystallization and purification of micafungin precursor FR901379, which solves the problem of difficulty and high cost of micafungin purification in the prior art from the source of raw materials

Method used

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  • Purification method of micafungin precursor fr901379
  • Purification method of micafungin precursor fr901379

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Add 5.5g of crude micafungin precursor FR901379 to a mixture of 12ml of water and 18ml of n-propanol, heat to 30°C and stir to dissolve, adjust the pH to 5.5 with formic acid, cool the solution to 5°C, and stir for 5 hours before filtering , dried in vacuo to obtain 2.0 g of purified micafungin precursor FR901379 whose purity meets the requirements, the purity determined by HPLC is 95.23%, and the main peak and the size of impurities are shown in the table below.

[0038] name main peak Impurity 1 Impurity 2 Impurity 3 Impurity 4 relative retention time 1.0 0.85 0.97 1.15 1.24 content% 95.74 0.33 0.91 0.26 0.77

Embodiment 2

[0040] Add 7.5g of crude micafungin precursor FR901379 to 12ml of water and 12ml of n-propanol mixture, heat to 40°C and stir to dissolve, use calcium acetate and sodium dihydrogen phosphate to adjust pH to 5.5, cool the solution to 25°C, continue Add 20ml of n-propanol, wait until the solution becomes turbid, stir at 25°C for 1 hour, then cool down to 15°C and stir for 3 hours, filter, and dry in vacuum to obtain 3.1g of purified micafungin precursor FR901379 with a purity that meets the requirements, HPLC The measured purity is 97.73%, and the main peak and the size of impurities are shown in the table below.

[0041] name main peak Impurity 1 Impurity 2 Impurity 3 Impurity 4 relative retention time 1.0 0.85 0.97 1.15 1.24 content% 97.73 0.23 0.34 0.23 0.55

Embodiment 3

[0043] Preparation of high-purity formula I compounds

[0044] Add 2.0g of crude micafungin precursor FR901379 to a mixture of 10ml of water and 10ml of n-propanol, heat to 40°C and stir to dissolve, adjust the pH to 5.0 with potassium acetate and potassium dihydrogen phosphate, cool the solution to 25°C, continue Add 20ml of n-propanol, wait until the solution becomes turbid, stir at 25°C for 1 hour, then cool down to 15°C and stir for 3 hours, filter, and dry in vacuum to obtain 1.7g of purified micafungin precursor FR901379 with a purity that meets the requirements, HPLC The measured purity is 98.21%. The main peak and the size of impurities are shown in the table below.

[0045] name main peak Impurity 1 Impurity 2 Impurity 3 Impurity 4 relative retention time 1.0 0.85 0.97 1.15 1.24 content% 98.21 0.17 0.22 0.14 0.47

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Abstract

The invention discloses a method for purifying micafungin precursors PR901379. The method includes steps of A, heating crude products of the micafungin precursors PR901379 according to certain concentration or dissolving the crude products in water or aqueous solution with organic solvents at the normal temperature and controlling the pH (potential of hydrogen) of dissolved liquid by the aid of alkali or acid solution; B, cooling the dissolved liquid to obtain the purified micafungin precursors PR901379 or adding organic solvents into the dissolved liquid to obtain the purified micafungin precursors PR901379; repeatedly carrying out the steps A and B as needed until the purified micafungin precursors PR901379 with the purity meeting requirements are obtained. The method has the advantages that the content of impurities in the micafungin precursors PR901379 is controlled by the aid of the low-toxicity solvents and the simple operation steps, and accordingly the high-purity micafungin precursors PR901379 can be obtained; the method is suitable for industrial production, and basic materials which are low in cost, excellent in quality and high in purity can be provided for synthesizing micafungin.

Description

technical field [0001] The invention relates to a method for treating chemical substances, in particular to a method for purifying micafungin precursor FR901379. Background technique [0002] Fungal infection has become the main reason for the high morbidity and mortality of infected patients, especially in recent years, with the continuous emergence of drug-resistant bacteria, the incidence of fungal infection continues to increase. Some critically ill patients and patients who have undergone major operations have become high-risk groups for fungal infections. [0003] Echinocandins, as a new antifungal drug, are effective in the treatment of infections caused by Candida or Aspergillus. This class of drugs is represented by caspofungin and micafungin, which inhibit 1,3 -Synthesis of β-glucosidic bonds, thereby inhibiting the reproduction of fungi, reducing and reducing the risk of infection for patients, and at the same time, because of the small side effects, it is widely...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07K7/56C07K1/30
CPCC07K7/56
Inventor 朱辉范雪涛张翠英韩晓彤杨益
Owner CHENGDU YATU BIOLOGICAL TECH