Preparation method of tilmicosin

A technology of tilmicosin and tylosin phosphate, which is applied to the preparation of sugar derivatives, chemical instruments and methods, sugar derivatives, etc., can solve the problems of large yield loss of tilmicosin, difficulty in industrial production, and application problems. The scope is limited and other problems, and the production process is easy to control, the production safety is high, and the preparation process is simple.

Active Publication Date: 2012-03-21
QILU ANIMAL HEALTH PROD +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The disadvantage of this preparation method is: it needs to go through multiple acid-base phase inversion extractions, so that the yield loss of tilmicosin is relatively large, the general yield is betwe

Method used

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  • Preparation method of tilmicosin

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preparation example Construction

[0013] A kind of preparation method of tilmicosin according to the present invention, take tylosin phosphate as raw material, alcohol as solvent, anhydrous formic acid as catalyst and 3,5-dimethylpiperidine at 65-97°C After the reaction is complete, the intermediate 20-dihydro-20-deoxy-(3,5-dimethylpiperidin-1-yl) tylosin is obtained, the solvent is concentrated, and the residue is hydrolyzed by adding 0.1N sulfuric acid solution to obtain substituted Micoxin, the mass volume ratio of tylosin phosphate to alcohol is 1:2-10, the mass ratio of tylosin phosphate to 3,5-dimethylpiperidine to anhydrous formic acid is 1:0.11-0.17 :5.6-8, the mass volume ratio of tylosin phosphate to 0.1N sulfuric acid solution is 1:2-6, the reaction formula is as follows:

[0014]

[0015] The preparation method of tilmicosin of the present invention can have the following various embodiments.

Embodiment 1

[0017] The specific steps of the preparation method of tilmicosin of the present invention are as follows:

[0018] ①Take 100kg of tylosin phosphate, put it into a reaction kettle, add 600L of methanol, heat up to reflux, stir and dissolve, and obtain a solution;

[0019] ② Take 8 kg of anhydrous formic acid and add 50 L of methanol to dissolve, and obtain a mixed solution for later use;

[0020] 3. Add 17kg of 3,5-dimethylpiperidine to the dissolving solution of step 1., then dropwise add the mixed solution of step 2., react at methanol reflux temperature for 4-5 hours until complete, and concentrate methanol in vacuo to obtain intermediate 20 -Dihydro-20-deoxy-(3,5-dimethylpiperidin-1-yl)tylosin liquid;

[0021] ④Add 400L of 0.1N sulfuric acid solution to the liquid intermediate 20-dihydro-20-deoxy-(3,5-dimethylpiperidin-1-yl)tylosin, and react at 50°C for 1 hour, Then 50 L of 2N sodium hydroxide was added dropwise to adjust the base to separate out tilmicosin. After filtr...

Embodiment 2

[0023] The specific steps of the preparation method of tilmicosin of the present invention are:

[0024] ①Take 100kg of tylosin phosphate, put it into a reaction kettle, add 200L of methanol, heat up to reflux, stir and dissolve, and obtain a solution;

[0025] ② Take 6.8kg of anhydrous formic acid and add 50L of methanol to dissolve, and obtain a mixed solution after dissolution;

[0026] 3. Add 14kg of 3,5-dimethylpiperidine to the dissolving solution of step 1., then dropwise add the mixed solution of step 2., react at methanol reflux temperature for 5-5.5 hours until complete, and concentrate methanol in vacuo to obtain intermediate 20 -Dihydro-20-deoxy-(3,5-dimethylpiperidin-1-yl)tylosin liquid;

[0027] ④Add 400L of 0.1N sulfuric acid solution to the liquid intermediate 20-dihydro-20-deoxy-(3,5-dimethylpiperidin-1-yl)tylosin, and react at 50°C for 1 hour, Then 50 L of 2N sodium hydroxide was added dropwise to adjust the base to separate out tilmicosin. After filtration...

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Abstract

The invention discloses a preparation method of tilmicosin. The method comprises the following steps of: reacting tylosin phosphate serving as a raw material with 3,5-lupetidine by taking alcohol as a solvent and taking anhydrous formic acid as a catalyst at 65-97 DEG C to obtain 20-dihydro-20-deoxy-(3,5-lupetidine-1-radical)tylosin serving as an intermediate; concentrating the solvent; and adding residues into 0.1N sulfuric acid solution for hydrolyzing to obtain tilmicosin, wherein the mass volume ratio of the tylosin phosphate to the alcohol is 1:(2-10), the mass ratio of the tylosin phosphate to the 3,5-lupetidine to the anhydrous formic acid is 1:(0.11-0.17):(5.6-8), and the mass volume ratio of the tylosin phosphate to the 0.1N sulfuric acid solution is 1:(2-6). The reaction formula is shown in the specifications. By adopting the method, the defects of the prior art can be overcome. The method is easy to control, and has high yield and low production cost.

Description

technical field [0001] The invention relates to a preparation method of veterinary medicine, which is a preparation method of tilmicosin. Background technique [0002] Tilmicosin is a special antibiotic drug for livestock and poultry. It is mainly used for the prevention and treatment of livestock pneumonia, avian mycoplasma disease and mastitis of lactating animals. At present, the method for preparing tilmicosin is to use tylosin phosphate or tartaric acid as raw material, hydrolyze under water-soluble acidic conditions, and then use non-water-soluble organic solvents such as amyl acetate, ethyl acetate or dichloromethane Alkali adjustment and extraction, the organic layer is extracted and formic acid is added, and 3,5-dimethylpiperidine is reacted to generate tilmicosin. The disadvantage of this preparation method is: it needs to go through multiple acid-base phase inversion extractions, so that the yield loss of tilmicosin is relatively large, the general yield is betw...

Claims

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Application Information

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IPC IPC(8): C07H17/08C07H1/00
Inventor 方明峰宁述群刘全才孔梅吴连勇
Owner QILU ANIMAL HEALTH PROD
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