Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

Refining method of tiamulin hydrogen fumarate

A technology of tiamulin fumarate and a refining method, which is applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., and can solve problems such as poor impurity removal effect, low solubility of tiamulin fumarate, and low utilization rate of equipment, etc. problems, to achieve the effects of saving production costs, improving equipment utilization, and improving product quality

Inactive Publication Date: 2011-05-25
ANHUI WANBEI PHARMA
View PDF1 Cites 3 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, most pharmaceutical industry adopts the method of ethyl acetate heavy crystal product, and the problem that this method exists is that the solubility of tiamulin fumarate in ethyl acetate is low (almost insoluble at normal temperature), needs a large amount of ethyl acetate solvent and relatively High temperature (about 78°C) can make it completely dissolved, the effect of impurity removal is poor, and the utilization rate of equipment is low

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] a, get 200g of tiamulin fumarate crude product, add 788g acetone;

[0017] b. While stirring, the temperature is raised to 55-57°C, the stirring speed is 35-45rpm, and the temperature is kept at reflux for 3-5 hours;

[0018] c. Lower the temperature at a rate of 8-10°C / h, and reduce the stirring speed to 18-22rpm to produce reflux crystallization;

[0019] d. When the temperature is lowered to 48°C, add an appropriate amount of tiamulin fumarate seed crystals, and when the temperature is lowered to 1°C, keep it warm for 2 to 3 hours to fully crystallize it;

[0020] e. Suction filtration by suction filter until no filtrate drips out, add 300g of cold acetone to wash twice, remove impurities and then drain to produce tiamulin fumarate fine powder;

[0021] f. Put the above fine powder into a vacuum drying oven, heat up to 55-65°C at a rate of 6°C / h, vacuum degree - (0.07-0.09) Mpa, and dry for 2-4 hours to obtain refined tiamulin fumarate powder .

[0022] After the ...

Embodiment 2

[0026] a, get tiamulin fumarate crude product 500g, add 1970g acetone;

[0027] b. While stirring, the temperature is raised to 55-57°C, the stirring speed is 35-45rpm, and the temperature is kept at reflux for 3-5 hours;

[0028] c. Lower the temperature at a rate of 8-10°C / h, and reduce the stirring speed to 18-22rpm to produce reflux crystallization;

[0029] d. When the temperature is lowered to 48°C, add an appropriate amount of tiamulin fumarate seed crystals, and when the temperature is lowered to 1°C, keep it warm for 2 to 3 hours to fully crystallize it;

[0030] e. Suction filtration by suction filter until no filtrate drips out, add 378g of cold acetone to wash twice, remove impurities and then drain to generate tiamulin fumarate fine powder;

[0031] f. Put the above fine powder into a vacuum drying oven, heat up to 55-65°C at a rate of 6°C / h, vacuum degree - (0.07-0.09) Mpa, and dry for 2-4 hours to obtain refined tiamulin fumarate powder .

[0032] After the r...

Embodiment 3

[0036] a, take tiamulin fumarate crude product 800g, add 3152g;

[0037] b. While stirring, the temperature is raised to 55-57°C, the stirring speed is 35-45rpm, and the temperature is kept at reflux for 3-5 hours;

[0038] c. Lower the temperature at a rate of 8-10°C / h, and reduce the stirring speed to 18-22rpm to produce reflux crystallization;

[0039] d. When the temperature is lowered to 48°C, add an appropriate amount of tiamulin fumarate seed crystals, and when the temperature is lowered to 1°C, keep it warm for 2 to 3 hours to fully crystallize it;

[0040] e. Suction filtration by suction filter until no filtrate drips out, add 512g of cold acetone to wash twice, remove impurities and then drain to generate tiamulin fumarate fine powder;

[0041] f. Put the above fine powder into a vacuum drying oven, heat up to 55-65°C at a rate of 6°C / h, and vacuum (0.07-0.09) Mpa, dry for 2-4 hours to obtain refined tiamulin fumarate powder.

[0042] After the refining is complet...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

The invention relates to a refining method of tiamulin hydrogen fumarate. The method is characterized by comprising the following steps: taking crude tiamulin hydrogen fumarate, adding crude tiamulin hydrogen fumarate in acetone in a weight ratio of 1:3-4; stirring at 35-45rpm while heating to 55-57 DEG C, refluxing for 3-5h while keeping the temperature; reducing the temperature at 8-10 DEG C / h, reducing the stirring speed to 18-22rpm, refluxing for crystallization; adding a defined amount of tiamulin hydrogen fumarate seed crystals when the temperature is reduced to 48 DEG C, keeping the temperature for 2-3h when the temperature is reduced to 1 DEG C to perform complete crystallization; performing suction filtering with a suction filtering machine to ensure that no filtrate drops, adding a defined amount of cold acetone to wash twice, removing impurities to draw off water and generate the refined tiamulin hydrogen fumarate powder; and placing the refined powder in a vacuum drying oven, heating at 6 DEG C / h to 55-65 DEG C, and drying for 2-4h under the vacuum degree of -(0.07-0.09)MPa to obtain the refined tiamulin hydrogen fumarate raw powder. The invention utilizes the property of tiamulin hydrogen fumarate that tiamulin hydrogen fumarate is slightly soluble in acetone, thus the dosage of the refined solvent can be reduced, the consumption of solvent can be lowered, the production cost can be reduced, the impurities of the product can be reduced and the product quality can be greatly increased.

Description

technical field [0001] The invention belongs to the field of biopharmaceuticals, and relates to a method for refining dietin antibiotics for animals, more precisely, a method for refining tiamulin fumarate. technical background [0002] Tiamulin fumarate is a dietene animal-specific antibiotic, mainly used to prevent poultry, livestock respiratory diseases and animal growth promotion, and is one of the top ten veterinary antibiotics in the world. It inhibits the synthesis of microbial proteins by interfering with microbial nucleosomes, thereby achieving antibacterial effects. In particular, it has unique antibacterial effect on mycoplasma, spirochete and actinomycete pathogens. At present, there are not many manufacturers in the market, and the demand for the product is large, and the product is very effective in treating chicken chronic respiratory disease, swine mycoplasma pneumonia, haemophilus pleuropneumonia, and dysentery caused by Treponema in swine, so the supply ex...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Applications(China)
IPC IPC(8): C07C323/52C07C319/28
Inventor 惠舰孙冠中黄超王幸姚健刘瑞华朱立元李为全张文
Owner ANHUI WANBEI PHARMA
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com