Preparation method of tiamulin base

A technology of tiamulin and tiamulin, which is applied in the field of preparation of tiamulin, can solve the problems such as difficult control of salt-forming crystallization process, influence product quality, etc., achieves reduction of salt-forming crystallization steps, easy Large-scale industrial production, easy-to-operate effect

Inactive Publication Date: 2012-09-19
宁夏泰瑞制药股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Most pharmaceutical industries use this process to prepare tiamulin fumarate, but there are many defects in this pro

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] 1. Filtration of fermentation broth and drying of mycelia

[0026] Add 5-10% volume of water to the fermentation broth and stir, then filter through a plate and frame filter press, and dry the filter cake with air when it is filtered until there is basically no filtrate flowing out. Crush the filter cake and dry it with a flash evaporator, controlling the inlet air temperature at 150-160°C and the outlet air temperature at 90-100°C. Mycelium drying weight loss does not exceed 15 ~ 20%.

[0027] 2. Dried mycelia extraction, extraction and concentration

[0028] The dry mycelium of pleuromutilin was leached twice with methanol, the volume of methanol added for the first time was 5 times of the mass of dry mycelium, the volume of methanol added for the second time was 4 times of the mass of dry mycelium, and the two mixtures were combined. The secondary extract is concentrated in vacuum to 40-50% of the original volume.

[0029] Transfer the concentrated solution into a...

Embodiment 2

[0036] 1, fermentation broth filtration and mycelia drying steps are the same as in Example 1

[0037] 2. Dried mycelia extraction, extraction and concentration

[0038] The dry mycelium of pleuromutilin was leached twice with methanol, the volume of methanol added for the first time was 6 times the mass of dry mycelia, the volume of methanol added for the second time was 5 times of the mass of dry mycelium, and the two mixtures were combined. The secondary extract is concentrated in vacuum to 40-50% of the original volume.

[0039] Transfer the concentrated solution into an extraction tank, add acetone to extract twice, the volume of acetone added to the first extraction is 6 times the volume of the concentrated solution, and the volume of acetone added to the second extraction is 5 times the volume of the concentrated solution. After the extraction is finished, let stand to separate and separate, the water phase goes to waste water treatment, and the ketone phase is transfe...

Embodiment 3

[0044] 1, fermentation broth filtration and mycelia drying steps are the same as in Example 1

[0045] 2. Dried mycelia extraction, extraction and concentration

[0046] The dry mycelium of pleuromutilin was leached twice with methanol, the volume of methanol added for the first time was 7 times of the mass of dry mycelia, the volume of methanol added for the second time was 5 times of the mass of dry mycelia, and the two mixtures were combined. The secondary extract is concentrated in vacuum to 40-50% of the original volume.

[0047] Transfer the concentrated solution into an extraction tank, add acetone for extraction twice, the volume of acetone added in the first extraction is 7 times the volume of the concentrated solution, and the volume of acetone added in the second extraction is 5 times the volume of the concentrated solution. After the extraction is finished, let stand to separate and separate, the water phase goes to waste water treatment, and the ketone phase is t...

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PUM

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Abstract

The invention relates to a preparation method of tiamulin base. The preparation method includes: filtering pleuromulin fermentation broth, drying mycelium, performing leaching by using methanol as solvent, using acetone to extract leach liquor after vacuum concentration, concentrating extract, transferring concentrate into a synthetic reactor, adding paratoluensulfonyl chloride, allowing for synthetic reaction at pH of 11-12 and reaction temperature of 20-30 DEG C, allowing for standing and layering after complete reaction, adding tetrabutylammonium bromide and diethylaminoethyl mercaptide into ketone phase respectively , allowing for full reaction at pH of 9-10 and the reaction temperature of 50-60 DEG C, adding water for extraction, discarding aqueous phase, filtering the ketone phase, and reducing the original volume to 60-70% by vacuum concentration to obtain tiamulin base. The original process is improved, the salifying and crystallization process is omitted, the tiamulin base is used to produce preparations directly, and accordingly equipment investment cost and production cost are lowered, product quality is improved, and the content of tiamulin base reaches 80-90%. Organic solvents used in the preparation method are recyclable, environmental pollution is reduced, and the preparation method has promising development prospect.

Description

technical field [0001] The invention belongs to the technical field of biopharmaceuticals, in particular to a preparation method of tiamulin base. Background technique [0002] Tiamulin is a diterpene (pluromulin) antibiotic prepared by semi-synthesis after obtaining pleuromutilin by fermenting and culturing Pleurotus mutilus. Tiamulin is a new type of animal-specific antibiotics. It has good antibacterial activity against mycoplasma and some Gram-positive bacteria. It is by far the most effective antibiotic against Mycoplasma septicemia in chickens. At the same time, it has a strong effect on Staphylococcus aureus, Streptococcus, various mycoplasma and some spirochetes. [0003] At present, the main product on the market is the fumarate of tiamulin. Firstly, the pleuromutilin fermentation liquid is obtained by fermentation, and the pleuromutilin is extracted from the fermentation liquid. After sulfonation reaction, it is salted to obtain the fumaric acid tiamulin fumaricin...

Claims

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Application Information

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IPC IPC(8): C07C323/52C07C319/14
Inventor 王义周丽娜奇乃赵伯龙
Owner 宁夏泰瑞制药股份有限公司
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