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Preparation method of tigecycline

A technology of adding tigecycline in batches, which is applied in the preparation of organic compounds, carboxylic acid amide preparation, chemical instruments and methods, etc., can solve the problems of harsh reaction conditions, low product purity and low yield, and achieve the goal of preparing The effect of simple process, high product purity and high yield

Active Publication Date: 2013-04-17
ANHUI YOUCARE KAIYUE PHARMA
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Problems solved by technology

[0003] The preparation process of tigecycline in the prior art has many defects such as low yield, harsh reaction conditions, and low product purity.

Method used

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  • Preparation method of tigecycline
  • Preparation method of tigecycline
  • Preparation method of tigecycline

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Embodiment Construction

[0027] Below in conjunction with embodiment and attached figure 1 The present invention is further described.

[0028] 1., prepare formula (III) compound by formula (II) compound

[0029] In a reactor with mechanical stirring, add concentrated sulfuric acid (98%) 1900ml, stir, cool the reaction solution to -10~15°C, add minocycline hydrochloride (compound of formula (II)) 100g in batches, complete, Maintain the temperature and stir for 20 minutes; control the temperature at -10 to 0°C, and then add 290 g of potassium nitrate in batches. After the addition is complete, keep the temperature at 0 to 5°C and continue to stir for 3 hours. Slowly add the reaction solution dropwise into 5000ml of cooled diethyl ether, and control the temperature not to exceed 15°C. After the dropwise addition, continue to stir for 10 minutes, a large amount of light yellow solid precipitates, filter, wash the filter cake twice with cold ethanol, and drain , transferred to a vacuum drying oven at 30...

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Abstract

The invention relates to the technical field of medicine synthesis, in particular to a preparation method of tigecycline. The preparation method of the tigecycline comprises the following steps: adding 1,900 mL of concentrated sulfuric acid into a reactor, stirring, cooling to -10 to 15 DEG C, adding 100 g of a compound (II) in batches, and preserving heat and stirring for 20 minutes; controlling the temperature at -10 to 10 DEG C, adding 285-295 g of potassium nitrate in batches, keeping the temperature at 0-5 DEG C, and further stirring for 3-4 h; and slowly dripping a reaction solution into the cooled 4,950-5,050 mL of diethyl ether, controlling the temperature at 0-15 DEG C, further stirring for 10-15 minutes after dripping, separating out light yellow solid, filtering, eluting a filter cake with cold ethanol twice, draining, and drying to obtain a compound (III). The preparation method of the tigecycline is simple and quick in preparation process, relatively high in yield, relatively simple and quick in refining process and relatively high in product purity, and is applicable to industrial production; and by the preparation method of the tigecycline, the reaction time can be effectively shortened.

Description

technical field [0001] The invention relates to the technical field of drug synthesis, in particular to a preparation method of tigecycline. Background technique [0002] Tigecycline (Tigecycline), trade name TYGACILTM (developed by Wyeth Drug Company of the United States) is a new type of broad-spectrum active antibiotic for intravenous injection, which is also active against drug-resistant methicillin-resistant Staphylococcus aureus. The first drug in the aminotetracycline class, a new drug approved by the US Food and Drug Administration (FDA) in June 2005. [0003] The preparation process of tigecycline in the prior art mostly has defects such as low yield, harsh reaction conditions, and low product purity. Contents of the invention [0004] The present invention aims to overcome the technical problems existing in the above-mentioned prior art, and proposes a preparation method of tigecycline with high yield and convenient industrial production. [0005] The technical...

Claims

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Application Information

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IPC IPC(8): C07C237/26C07C231/02
Inventor 周如国
Owner ANHUI YOUCARE KAIYUE PHARMA
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