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Preparation method of methacycline

A technology of oxytetracycline and oxytetracycline, which is applied in the field of preparation of oxytetracycline methacycline, can solve the problems of rising cost of catalytic hydrogenation, high cost of oxytetracycline methacycline, and difficult control of catalyst activity , to achieve good industrialization prospects, reduce production costs, and mild reaction conditions

Active Publication Date: 2020-01-10
SHANDONG GUOBANG PHARMA +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This type of method has a relatively simple reaction type, but a large amount of sulfur-containing waste salt will be produced after the dechlorination of the reducing agent is completed. At present, the pressure on environmental protection is relatively high, wastewater treatment is difficult, and the industrialization cost is high; (2) the other type is based on soil 11α-chloro-6-methine oxytetracycline p-toluenesulfonate was prepared from oxytetracycline as the initial raw material, and methoxytetracycline was obtained by selective hydrogenation with hydrogen under pressure in the presence of heterogeneous catalyst palladium carbon. This type of method is the current mainstream method for preparing methoxytetracycline, but palladium and charcoal heterogeneous catalysts are difficult to control the catalyst activity during the catalytic dechlorination process, and the hydrogenation process is also easy to cause the dechlorination product methoxytetracycline Doxycycline is further hydrogenated into doxycycline, the reaction selectivity is low
In addition, the price of precious metal palladium has been rising in recent years, resulting in the rising cost of catalytic hydrogenation, and the cost of preparing the product methacycline is getting higher and higher.

Method used

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  • Preparation method of methacycline
  • Preparation method of methacycline
  • Preparation method of methacycline

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Add 300.34g of purified water into a 500ml reaction bottle equipped with a thermometer and mechanical stirring, add 30.02g of activated carbon with a specific surface area of ​​700-900㎡ / g, add dropwise 11.40ml of ruthenium trichloride aqueous solution with a concentration of 0.2g / ml, Heat and stir for 12 hours, put the impregnating solution into a 500ml autoclave, keep warm at 60°C, charge hydrogen and stir for 2.5 hours, and filter out 57.12g of wet catalyst.

[0028] Add 100.12g of solvent 50% ethanol water to a 500ml autoclave, drop into 20.03g of 11α-chloro-6methine oxytetracycline p-toluenesulfonate, keep warm at 15°C, drop into 0.78g of the ruthenium carbon catalyst prepared above, and charge hydrogen The reaction was stirred for 7 hours, and liquid phase analysis was carried out by sampling. The conversion rate was 71.2%, the selectivity was 98.4%, and the yield was 70.1%.

Embodiment 2

[0030] Drop into 50% ethanol water 100.23g as solvent in a 500ml autoclave, drop into 20.01g of 11α-chloro-6methine oxytetracycline p-toluenesulfonate, keep warm at 30°C, drop into the ruthenium carbon prepared in Example 1 Catalyst 0.74g, charged with hydrogen and stirred for 7 hours, sampling for liquid phase analysis, the conversion rate was 99.3%, the selectivity was 97.1%, and the yield was 96.4%.

Embodiment 3

[0032] In a 500ml autoclave, drop into solvent as 100.23g of 50% ethanol water, drop into 20.01g of 11α-chloro-6methine oxytetracycline p-toluenesulfonate, keep warm at 65°C, drop into the ruthenium carbon prepared in Example 1 Catalyst 0.75g, charged with hydrogen and stirred for 7 hours, liquid phase analysis by sampling, the conversion rate was 99.1%, the selectivity was 95.5%, and the yield was 94.7%.

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Abstract

The invention discloses a preparation method of methacycline. The method includes: firstly taking water as a solvent, adding a ruthenium precursor into a carrier activated carbon, carrying out hydrogenation activation to obtain a ruthenium-carbon catalyst, and hydrogenating the ruthenium-carbon catalyst for reaction with 11alpha-chloro-6-methenyl oxytetracycline p-toluenesulfonate to obtain methacycline. The method has the advantages of simple process, mild reaction conditions and high total yield, enhances the product selectivity, lowers the production cost, and avoids the generation of threewastes, thus having favorable industrial prospects.

Description

technical field [0001] The invention belongs to the technical field of veterinary drug production, in particular to a method for preparing methacycline. Background technique [0002] Methacycline, also known as metacycline, is a semi-synthetic tetracycline with broad-spectrum antibacterial activity, high-efficiency and long-lasting antibacterial activity. The antibacterial mechanism is the same as tetracycline, but the antibacterial effect is stronger than tetracycline. It has strong antibacterial activity against Gram-positive or negative bacteria; it can be used for rickettsiasis, mycoplasma pneumonia, lymphogranuloma, chancre, plague, cholera, brucellosis (combined application with streptomycin), etc. It is also effective against systemic or local infections caused by sensitive strains such as Escherichia coli, Bacillus aerogenes, Shigella, Haemophilus influenzae, and Klebsiella. In addition, for infections caused by Neisseria gonorrhoeae, Bacillus anthracis, Actinomyce...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C231/12C07C237/26B01J23/46
CPCC07C231/12B01J23/462C07C2603/46C07C237/26
Inventor 达先鹏廖仕学李芳郭兴龙王伟宏曲俊腾
Owner SHANDONG GUOBANG PHARMA
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