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Production method for improving quality of tilmicosin phosphate

A technology for tilmicosin phosphate and a production method, which is applied in chemical instruments and methods, sugar derivatives, sugar derivatives, etc., can solve the problems of high residual water content of butyl acetate, long operation time, influence on amination reaction and the like , to achieve the effect of shortening the time for butyl acetate to extract static water, reducing production man-hours and reducing impurities

Pending Publication Date: 2022-03-04
QILU PHARMA INNER MONGOLIA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The above two methods, before the amination, all use organic solvent extraction and natural stratification before amination. The operation time is long, and the residual water in the butyl acetate is large, which eventually leads to many impurities and low purity in the finished product; The entrainment of organic solvents will affect the amination reaction, further resulting in more impurities in the finished product

Method used

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  • Production method for improving quality of tilmicosin phosphate

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Embodiment 1

[0028] A production method improving the quality of tilmicosin phosphate, the method is as follows:

[0029] 1) Use butyl acetate as the extractant to perform countercurrent extraction on the tylosin tartrate concentrated solution, collect the extract, the volume ratio of the tylosin tartrate concentrated solution to butyl acetate is 10:4, and the extraction temperature is 45°C. pH control at 7.0;

[0030] 2) After adding butyl acetate for extraction, stand still for 35 min, discard the water phase, and obtain 5 m of butyl acetate extract 3 ;

[0031] 3) adding anhydrous sodium sulfate to the extract, stirring for 50 minutes, then filtering to remove anhydrous sodium sulfate, and then performing amination synthesis; the amount of anhydrous sodium sulfate added is 8.0% of the quality of the extract;

[0032] 4) Add 3,5-dimethylpiperidine, formic acid and ethyl acetate to the system for amination reaction, the molar ratio of tylosin to 3,5-dimethylpiperidine is 1:1; The molar...

Embodiment 2

[0035] A production method improving the quality of tilmicosin phosphate, the method is as follows:

[0036] 1) Use butyl acetate as the extractant to perform countercurrent extraction on the tylosin tartrate concentrated solution, collect the extract, the volume ratio of the tylosin tartrate concentrated solution to butyl acetate is 10:4.5, and the extraction temperature is 45°C. pH control at 7.0;

[0037] 2) After adding butyl acetate for extraction, stand still for 30 min, discard the water phase, and obtain 5 m of butyl acetate extract 3 ;

[0038] 3) adding anhydrous sodium sulfate to the extract, stirring for 40 minutes, then filtering to remove anhydrous sodium sulfate, and then performing amination synthesis; the amount of anhydrous sodium sulfate added is 10.0% of the quality of the extract;

[0039] 4) Add 3,5-dimethylpiperidine, formic acid and ethyl acetate to the system for amination reaction, the molar ratio of tylosin to 3,5-dimethylpiperidine is 1:1.5; Tylos...

Embodiment 3

[0042] A production method improving the quality of tilmicosin phosphate, the method is as follows:

[0043] 1) Use butyl acetate as the extractant to perform countercurrent extraction on the tylosin tartrate concentrated solution, collect the extract, the volume ratio of the tylosin tartrate concentrated solution to butyl acetate is 11:4.5, and the extraction temperature is 45°C. pH control at 7.0;

[0044] 2) After adding butyl acetate for extraction, stand still for 25 min, discard the water phase, and obtain 5 m of butyl acetate extract 3 ;

[0045] 3) adding anhydrous sodium sulfate to the extract, stirring for 45 minutes, then filtering to remove anhydrous sodium sulfate, and then performing amination synthesis; the amount of anhydrous sodium sulfate added is 7.0% of the mass of the extract;

[0046] 4) Add 3,5-dimethylpiperidine, formic acid and ethyl acetate to the system for amination reaction, the molar ratio of tylosin to 3,5-dimethylpiperidine is 1:1.5; Tylosin ...

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Abstract

The invention relates to a production method for improving the quality of tilmicosin phosphate, which is characterized in that anhydrous sodium sulfate is added into extract liquor for stirring treatment after butyl acetate extraction for 20-40 minutes and before amination synthesis, so that on one hand, the standing water separation time of butyl acetate extraction is greatly shortened, and the standing water separation time of the extraction in the original process needs 5-6 hours; and after the anhydrous sodium sulfate is added, the water separation time is 30-60 minutes, so that the production time is shortened. On the other hand, moisture in the extract liquor is greatly removed, and a specific amount of anhydrous sodium sulfate is added at a specific time, so that the moisture in the extract liquor is lower than 2.0%, the subsequent inadequate amination reaction is avoided, the amination reaction is thorough, the mass of tilmicosin phosphate is improved, and the total impurity content is reduced by 3.0%.

Description

technical field [0001] The invention relates to a production method for improving the quality of tilmicosin phosphate, which belongs to the technical field of biological veterinary drug preparation. Background technique [0002] Tilmicosin phosphate is a phosphate formed from Tilmicosin (Tilmicosin) and phosphoric acid. Cyclic lactone antibiotics for livestock and poultry, due to its special antibacterial activity and pharmacokinetic characteristics, the drug has been approved for clinical use in the prevention and treatment of infectious diseases in cattle, goats, sheep, dairy cows, pigs, chickens and other animals, especially Livestock and poultry respiratory diseases, such as livestock actinobacillus pleuropneumonia, pasteurellosis and chicken mycoplasma disease, etc., and the treatment of lactating animal mastitis; it has a similar molecular structure and antibacterial spectrum to tylosin, but it is effective for some The antibacterial activity of pathogenic bacteria is...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H1/00C07H1/06C07H17/08
CPCC07H1/00C07H1/06C07H17/08
Inventor 唐英彬马虎初翔飞
Owner QILU PHARMA INNER MONGOLIA
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