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Refining method of high-purity tigecycline

A technology for tigecycline and a purification method, which is applied in the separation/purification of carboxylic acid amides, bulk chemical production, organic chemistry, etc. The effect of preparation, good safety and cost reduction

Inactive Publication Date: 2018-06-01
HUNAN ER KANG PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method solves the problem that conventional purification methods require high purification conditions such as temperature and humidity, and is simple to operate, but this method requires the use of a large amount of organic solvents

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Put 100 g (0.171 mol) of crude tigecycline into a supercritical fluid extraction tank, add 100 mL of isopropyl acetate, set the extraction temperature to 30 °C, pressure to 10 Mpa, time to 30 min, and stirring speed to 100 rpm to obtain The purified product of tigecycline was 88 g, and the yield was 88%.

Embodiment 2

[0028] Put 100 g (0.171 mol) of crude tigecycline into a supercritical fluid extraction tank, add 100 ml of isopropyl acetate-acetone, set the extraction temperature to 25°C, pressure to 12 Mpa, time to 40 min, and stirring speed to 100 rpm. 79 g of the purified product of tigecycline was obtained, with a yield of 79%.

Embodiment 3

[0030] Put 100 g (0.171 mol) of crude tigecycline into a supercritical fluid extraction tank, add 100 mL of isopropyl acetate-methanol, set the extraction temperature to 30°C, pressure to 10 Mpa, time to 30 min, and stirring speed to 150 rpm , to obtain 85 g of purified product of tigecycline with a yield of 85%.

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PUM

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Abstract

The invention discloses a refining method of high-purity tigecycline. A crude tigecycline product is added to an extraction tank of a supercritical fluid extractor, an entrainer is added, after extraction, a mixed epimer is removed, and the high-purity tigecycline is obtained. The temperature and humidity are strictly required while the purification operation of tigecycline is guaranteed, and therefining method which causes few solvent residues, has high refining purity, is simple to operate and has a green and environment-friendly process is designed.

Description

technical field [0001] The present invention belongs to the field of medicinal chemistry, specifically a method for purifying tigecycline, more precisely (4S, 4aS, 5aR, 12aS)-9-(2-tert-butylaminoacetamido)-4,7-bis Dimethylamino-1,4,4a,5,5a,6,11,12a-octahydro-3,10,12,12a-tetrahydroxy-1,11-dioxo-2-tetracenecarboxamide Purification method. Background technique [0002] The English name of Tigecycline is Tigecycline, tygacil, alias 9-tert-butylglycylaminominocycline, Dingglyminocycline, chemical name (4S, 4aS, 5aR, 12aS)-9-(2-tert Butylaminoacetamido)-4,7-bisdimethylamino-1,4,4a,5,5a,6,11,12a-octahydro-3,10,12,12a-tetrahydroxy-1,11- Dioxo-2-tetracenecarboxamide. Tigecycline (Tigecycline) is a 9-tert-butylglycinamide minocycline derivative developed by Wyeth, which has a broad-spectrum antibacterial activity, and its antibacterial spectrum includes Gram-positive and Gram-positive Blue-negative aerobic bacteria and anaerobic bacteria and other important clinical isolates of pa...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C231/24C07C237/26
CPCC07C231/24C07C237/26Y02P20/54
Inventor 帅放文王向峰章家伟
Owner HUNAN ER KANG PHARMA