High purity cyclic peptide compound and preparation method and application thereof

A compound and high-purity technology, applied in the field of high-purity cyclic peptide compounds and their preparation, can solve the problems of a large number of organic solvents, low product purity, and difficulty in scaling up production.

Active Publication Date: 2012-08-08
SHANGHAI TECHWELL BIOPHARMACEUTICALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Wherein WO9611210 report adopts preparative column to carry out separation and preparation, but this method needs a large amount of organic solvents, causes serious pollution to environment, is difficult for scale-up production; And the purity of obtained product is not high
WO03018615 and WO2004014879 use crystallization method for purification, but the result of crystallization cannot effectively remove impurity 6, impurity 7, impurity 8, impurity 9 and impurity 10

Method used

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  • High purity cyclic peptide compound and preparation method and application thereof
  • High purity cyclic peptide compound and preparation method and application thereof
  • High purity cyclic peptide compound and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0296] Preparation of crude compound I

[0297] Referring to the method of Example 1 of US Patent No. 5,376,634, 76 g of solid powder of Compound I was prepared, and the content determined by HPLC was 97.51%, see figure 1 HPLC analysis spectrum.

[0298] Table 1

[0299] Impurity name

Embodiment 2

[0301] Preparation of high-purity formula I compound

[0302] At 30° C., 3.6 g of the crude compound I prepared in Example 1 was dissolved in a mixed solution of 25 ml of water and 20 ml of n-propanol, and stirred to completely dissolve the compound I. Glacial acetic acid was used to adjust the pH to 3.5, and the solution was cooled to 15°C, the crystals of Compound I were precipitated, and the stirring was continued at 15°C for 5 hours, so that the crystals of Compound I gradually grew. 90 ml of n-propanol was added dropwise, and after completion of the dropwise addition, the mixture was stirred at 15° C. for 1 hour. Suction filtration and vacuum drying afforded 3.5 g of compound I with a purity of 99.00% as determined by HPLC. The contents of the main relevant impurities are shown in Table 2.

[0303] Table 2

[0304] Impurity name

Embodiment 3

[0306] Preparation of high-purity formula I compound

[0307] At 40°C, 3.5g of Compound I prepared in Example 2 (Compound I prepared in Example 2, with an HPLC purity of 99.00%) was dissolved in a mixed solution of 19ml of water and 16ml of n-propanol, and stirred to make the compound I dissolve completely. Glacial acetic acid was used to adjust the pH to 2.0, and the solution was cooled to 15°C, the crystals of compound I were precipitated, and the stirring was continued at 15°C for 5 hours, so that the crystals of compound I grew gradually. 70 ml of n-propanol was added dropwise, and after the dropwise addition was completed, the mixture was stirred at 15° C. for 1 hour. Suction filtration and vacuum drying afforded 3.4 g of compound I with a purity of 99.23% as determined by HPLC. The content of relevant impurities is shown in Table 3.

[0308] table 3

[0309] Impurity name

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Abstract

The invention discloses a high purity cyclic peptide compound, and a chemical structure is illustrated in formula I. R represents H or a cation ion capable of forming salt acceptable in pharmacy, and the purity is larger than and equal to 99.0%. A preparation method and application of the high purity cyclic peptide compound are further disclosed.

Description

technical field [0001] The present invention relates to a high-purity cyclic peptide compound and a preparation method thereof, and also relates to the use of the high-purity cyclic peptide compound. Background technique [0002] Fungal infection has become the main cause of high morbidity and mortality in immunocompromised patients. The incidence of fungal infections has increased significantly over the past 20 years. High-risk groups for fungal infections include critically ill patients, surgical patients, and those with HIV infection, leukemia, and other neoplastic diseases. Those who have undergone organ transplantation are also at high risk of fungal infection. [0003] Echinocandins, a new class of antifungal drugs, are effective in the treatment of infections caused by Candida or Aspergillus. This class of drugs is represented by caspofungin and micafungin. Echinocandin drugs inhibit fungi by inhibiting the formation of 1,3-β glycosidic bonds, thereby better reduc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07K7/56A61K38/12A61P31/10
CPCC07K7/56A61K38/12A61K38/00A61P31/10C07K1/16C07K1/306C07K1/30C07K1/34C07K1/36
Inventor 刘石东张兆利王修胜张晓焦广俊何兵明唐志军季晓铭
Owner SHANGHAI TECHWELL BIOPHARMACEUTICALS CO LTD
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