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A kind of preparation method of capreomycin

A capreomycin and resin technology, applied in the field of preparation of capreomycin, can solve problems such as difficulty in separation and purification

Inactive Publication Date: 2015-07-29
HYBIO PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] At present, capreomycin is mainly biosynthesized, and this method will inevitably produce two by-products of capreomycin IIA or IIB, making separation and purification difficult

Method used

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  • A kind of preparation method of capreomycin
  • A kind of preparation method of capreomycin
  • A kind of preparation method of capreomycin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] Embodiment 1: the synthesis of Fmoc-Ser (tBu)-CTC resin

[0043] Weigh 100 g of 2-CTC resin with a substitution degree of 0.1 mmol / g, add it to a solid-phase reaction column, wash it twice with an appropriate amount of DMF, and then use 300 ml of DMF to swell the resin for 30 minutes. Dissolve 11.5g of Fmoc-Ser(tBu)-OH in 60ml of DMF, add 10.5mL of DIPEA under an ice-water bath, then add the mixture into the above-mentioned reaction column filled with resin, and react at room temperature for 2 hours. Then add 8 mL of anhydrous methanol to seal for 1 hour, wash with appropriate amount of DMF 3 times, appropriate amount of DCM for 3 times, then seal with appropriate amount of anhydrous methanol for 30 minutes, and shrink the resin by draining methanol to obtain Fmoc-Ser(tBu)-CTC Resin, detection substitution degree is 0.081mmol / g.

Embodiment 2

[0044] Embodiment 2: the synthesis of Fmoc-Ser (tBu)-CTC resin

[0045] Weigh 20 g of 2-CTC resin with a substitution degree of 0.5 mmol / g, add it to a solid-phase reaction column, wash it twice with an appropriate amount of DMF, and then use 60 ml of DMF to swell the resin for 30 minutes. Dissolve 11.5g of Fmoc-Ser(tBu)-OH in 60ml of DMF, add 10.5mL of DIPEA under an ice-water bath, then add the mixture into the above-mentioned reaction column filled with resin, and react at room temperature for 2 hours. Then add 8 mL of anhydrous methanol to seal for 1 hour, wash with appropriate amount of DMF 3 times, appropriate amount of DCM for 3 times, then seal with appropriate amount of anhydrous methanol for 30 minutes, and shrink the resin by draining methanol to obtain Fmoc-Ser(tBu)-CTC Resin, detection substitution degree is 0.412mmol / g.

Embodiment 3

[0046] Embodiment 3: the synthesis of Fmoc-Ser (tBu)-CTC resin

[0047] Weigh 10 g of 2-CTC resin with a substitution degree of 1.0 mmol / g, add it to a solid-phase reaction column, wash it twice with an appropriate amount of DMF, and then use 30 ml of DMF to swell the resin for 30 minutes. Dissolve 11.5g of Fmoc-Ser(tBu)-OH in 60ml of DMF, add 10.5mL of DIPEA under an ice-water bath, then add the mixture into the above-mentioned reaction column filled with resin, and react at room temperature for 2 hours. Then add 8 mL of anhydrous methanol to seal for 1 hour, wash with appropriate amount of DMF 3 times, appropriate amount of DCM for 3 times, then seal with appropriate amount of anhydrous methanol for 30 minutes, and shrink the resin by draining methanol to obtain Fmoc-Ser(tBu)-CTC Resin, detection substitution degree is 0.834mmol / g.

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Abstract

The invention relates to a preparation method of capreomycin and particularly to a method for solid-phase synthesis capreomycin. The method comprises the following steps: enabling Fmoc-Ser(tBu)-OH or Fmoc-Ala-OH to react in a solvent with resin in presence of an organic base to generate Fmoc-Ser(tBu)-resin or Fmoc-Ala-resin, obtaining linear full-protection resin through deprotection and a coupling step, and then obtaining the required product through pyrolysis, ring formation and deprotection.

Description

technical field [0001] The invention relates to a method for preparing capreomycin, in particular to a method for solid-phase synthesis of capreomycin. Background technique [0002] [0003] Capreomycin is a basic cyclic polypeptide isolated from Streptomyces St r. its subcomponents. Capreomycin has antibacterial effect on mycobacterium tuberculosis and some non-tuberculous mycobacteria (such as Mycobacterium kansasii), and its minimum inhibitory concentration (MIC) is about 10 μg / ml, which can easily reach a high blood concentration and can be used to treat other mycobacteria. Tuberculosis patients whose pathogenic bacteria are resistant to other less toxic drugs. [0004] At present, capreomycin is mainly biosynthesized, and this method inevitably produces two by-products of capreomycin IIA or IIB, which makes separation and purification difficult. Contents of the invention [0005] In order to selectively synthesize capreomycin IA or IB, the invention provides a m...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07K7/56C07K1/06C07K1/04
CPCY02P20/55
Inventor 陈友金刘建马亚平袁建成
Owner HYBIO PHARMA