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Preparationmethod of macrolide compound

A technology of macrolides and compounds, applied in the field of biochemistry

Active Publication Date: 2015-04-08
NCPC NEW DRUG RES & DEV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] In the current research, the research on OP-1118 is concentrated in the research field of its antibacterial activity, but few people have conducted in-depth discussion and research on the preparation method of OP-1118

Method used

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  • Preparationmethod of macrolide compound
  • Preparationmethod of macrolide compound
  • Preparationmethod of macrolide compound

Examples

Experimental program
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Effect test

Embodiment 1

[0026] a. Disperse 1 g of fidaxomicin coarse powder in 10 ml of 0.1 mol / L NaOH aqueous solution, react at 20°C for 24 hours, filter, wash with distilled water, and filter under reduced pressure to obtain 0.9 g of OP-1118 coarse powder.

[0027] b. Add 3ml of acetonitrile to the OP-1118 coarse powder, sonicate for 2 minutes, and filter with a 0.45 μm filter membrane to obtain the sample solution.

[0028] c. Inject the sample solution into a medium-pressure chromatography column equipped with 90ml ODS, add acetonitrile:acid water mixed solution for elution, the ratio of trifluoroacetic acid and water in acid water is 5:10000 (v / v), HPLC On-line detection, collect the eluate with content ≥98.5%, concentrate to dryness under reduced pressure at 30°C to obtain 0.5g solid, add 5ml of crystallization solvent composed of acetonitrile and water with a volume ratio of 4:1, heat to dissolve, and then slowly cool down At 2°C, crystallize for 14 hours, and filter with suction to obtain OP...

Embodiment 2

[0033] a. Disperse 3 g of fidaxomicin coarse powder in 30 ml of 0.15 mol / L NaOH aqueous solution, react at 10°C for 48 h, filter, wash with distilled water, and filter under reduced pressure to obtain 2.6 g of OP-1118 coarse powder.

[0034] b. Add 15ml of methanol to the OP-1118 coarse powder, sonicate for 5 minutes, and filter with a 0.45 μm filter membrane to obtain the sample solution.

[0035] c. Inject the sample solution into a medium-pressure chromatography column equipped with 130ml ODS, add a mixed solution of methanol:acid water for elution, the ratio of acetic acid and water in acid water is 1:5000 (v / v), HPLC online detection , collect the eluent with content ≥98.5%, concentrate to dryness under reduced pressure at 40°C to obtain 1.4g solid, add 7ml of crystallization solvent composed of methanol and water with a volume ratio of 4:1, heat to dissolve, and slowly cool down to 5 ℃, crystallized for 20 hours, and filtered with suction to obtain OP-1118 crystalline po...

Embodiment 3

[0037] a. Disperse 5 g of fidaxomicin coarse powder in 50 ml of 0.2 mol / L NaOH aqueous solution, react at 30°C for 12 hours, filter, wash with distilled water, and filter under reduced pressure to obtain 4.6 g of OP-1118 coarse powder.

[0038] b. Add 20ml of ethanol to the OP-1118 coarse powder, sonicate for 5 minutes, and filter with a 0.45 μm filter membrane to obtain the sample solution.

[0039]c. Inject the sample solution into a medium-pressure chromatography column equipped with 320ml ODS, add ethanol: acid water mixed solution for elution, the ratio of acetic acid and water in acid water is 3:10000 (v / v), HPLC online detection , collect the eluent with content ≥98.5%, concentrate to dryness under reduced pressure at 50°C to obtain 2.5g of solid, add 37ml of crystallization solvent composed of ethyl acetate and ethanol with a volume ratio of 1:10, heat to dissolve, and then slowly cool down to 10°C, crystallize for 28 hours, and filter with suction to obtain OP-1118 cr...

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Abstract

The invention discloses a preparation method of a macrolide compound OP-1118. The method comprises the following steps: a, reacting fidaxomicin in alkaline solution to obtain a reaction product; b, dissolving the reaction product obtained in the step a in an organic solvent to obtain a sample liquid; and c, conducting chromatography on the sample solution in a C18 medium pressure column to obtain a macrolide compound OP-1118 with purity more than 98.5%. The preparation method of the invention has the advantages of simple operation and high sample recovery rate, and is applicable to industrialization production.

Description

technical field [0001] The invention belongs to the technical field of biochemistry, and relates to a preparation method of macrolide compounds, more precisely, to a preparation method of OP-1118. Background technique [0002] Fidaxomicin, also known as fidaxomicin, developed by Optimer, is a macrolide antibiotic with an 18-membered ring structure produced by the fermentation of Actinomycetes mobilis, belonging to a narrow-spectrum type Antibacterial drugs have excellent antibacterial effects on Gram-positive aerobic and anaerobic bacteria. They mainly produce rapid anti-refractory Clostridium infection (CDI) effects by inhibiting bacterial RNA polymerase, and are excellent in the treatment of CDI. to existing vancomycin. Fidaxomicin is mainly used clinically for the treatment of diseases caused by Clostridium difficile infection. It has the advantages of low tendency to develop resistance, long-lasting post-antibiotic effect, low cross-resistance and few adverse reactions....

Claims

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Application Information

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IPC IPC(8): C07H17/08C07H1/00
CPCC07H1/00C07H17/08
Inventor 张雪霞李晓露任风芝马瑛可爱兵王海燕高月麒段宝玲
Owner NCPC NEW DRUG RES & DEV
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