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Preparation method of tilmicosin

A technology of tilmicosin and substances, which is applied in the preparation of sugar derivatives, chemical instruments and methods, sugar derivatives, etc., can solve the problems of easy doping of catalysts and low purity, and achieve reduced reaction time, high purity, and improved The effect of production efficiency

Pending Publication Date: 2020-06-12
ZHEJIANG KANGMU PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The present invention aims to overcome the defect that the preparation method of tilmicosin in the prior art needs to use more catalysts, and at the same time, the catalyst is easily doped into the product resulting in low purity, and provides a method for synthesizing tilmicosin without a catalyst. The preparation method of star, this method can also effectively improve the purity of tilmicosin

Method used

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  • Preparation method of tilmicosin
  • Preparation method of tilmicosin
  • Preparation method of tilmicosin

Examples

Experimental program
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Effect test

Embodiment 1

[0028] Add 200g of water to a 500ml flask, add 50g of tylosin tartrate, stir and heat up to 20°C to dissolve, then add liquid caustic soda dropwise, adjust the pH to 8, add 200ml of butyl acetate for extraction, dehydrate the organic layer with 10g of sodium sulfate, add 8g of 3,5-dimethylpiperidine was kept at 50°C for 2 hours, and after that, the temperature was lowered to 30°C and 2.4g of sodium borohydride was added to react at 80°C for 2 hours. After completion, add sulfuric acid aqueous solution dropwise, adjust PH=1, react for 2 hours, complete, separate layers, add sodium hydroxide solution dropwise to the water layer, adjust PH=8, precipitate, filter, wash with water, and dry to obtain tilmicol star. Mass 41g, yield: 82%.

[0029] The prepared tilmicosin was tested for content, and the test conditions were as follows: use octadecylsilane bonded silica gel as filler; use water-acetonitrile-dibutylamine phosphate solution [get 16.8ml of dibutylamine, add phosphoric aci...

Embodiment 2

[0033] Add 500g of water to a 1000ml flask, add 80g of tylosin tartrate, stir and heat up to 40°C to dissolve, then add liquid caustic soda dropwise, adjust the pH to 11, add 350ml of chloroform for extraction, dehydrate the organic layer with 20g of sodium sulfate, add 3, 8.6g of 5-dimethylpiperidine was kept at 40°C for 2 hours. After completion, the temperature was lowered to 10°C and 4.1g of potassium borohydride was added to react for 2 hours. After completion, add sulfuric acid solution dropwise, adjust PH=3, react for 2 hours, complete, separate layers, add sodium hydroxide solution dropwise to the water layer, adjust PH=11, precipitate, filter, wash with water, and dry to obtain tilmicol star. Mass 56.2g, yield: 85%, content 96.3%.

Embodiment 3

[0035] Add 200g of water to a 1000ml flask, add 60g of tylosin tartrate, stir and heat up to 30°C to dissolve, then add liquid caustic soda dropwise, adjust the pH to 10, add 350ml of butyl acetate for extraction, dehydrate the organic layer with 10g of sodium sulfate, add 16.1 g of 3,5-dimethylpiperidine was kept at 65°C for 1.5 hours. After completion, the temperature was lowered to -10°C and 25.1 g of diethylmethoxyborane was added to react for 2 hours. After completion, add sulfuric acid solution dropwise, adjust PH=2, react for 2 hours, complete, separate layers, add sodium hydroxide solution dropwise to the water layer, adjust PH=9, precipitate, filter, wash with water, and dry to obtain tilmicol star. Mass 56.2g, yield: 85%, content 96.1%.

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Abstract

The invention relates to the field of pharmaceutical engineering, and particularly relates to a preparation method of tilmicosin. The preparation method comprises the following steps: taking tylosin tartrate and 3, 5-dimethylpiperidine as raw materials under a certain temperature condition, and enabling the tylosin tartrate and the 3, 5-dimethylpiperidine to generate a Mannich condensation reaction in a polar solvent medium to obtain an intermediate state substance; reducing the intermediate state substance to obtain an intermediate; and desugaring the intermediate to obtain tilmicosin. The preparation method overcomes defects that the tilmicosin preparation method in the prior art needs more catalysts, and the catalysts are easily doped into a product to cause lower purity. Therefore, compared with the prior art, in the invention, different synthesis routes are adopted, and the tilmicosin can be efficiently synthesized under a condition of omitting the catalysts; meanwhile, reaction time is effectively shortened so that production efficiency of tilmicosin is improved, and the purity of the synthesized tilmicosin is higher.

Description

technical field [0001] The invention relates to the field of pharmaceutical engineering, in particular to a preparation method of tilmicosin. Background technique [0002] Tilmicosin is a relatively new macrolide semi-synthesized antibiotic for livestock and poultry from tylosin, and its chemical name is 4A-O-de(2,6-dideoxy-3-C-methyl -L-ribose-pyranylhexyl)-20-deoxy-20-(3,5-dimethyl-1-piperidinyl)-[20(cis:trans)]tylosin, molecular formula C 46 h 80 N 2 o 13 , molecular weight 869.15. The antibacterial spectrum of tilmicosin is similar to that of tylosin, but it has enhanced effect against Pasteurella multocida and Pasteurella hemolytica. It was successfully developed in the 1980s, initially using Chemicalbook EL-870 as the code name, and its preparations include tilmicosin soluble powder, premix (20%), and injection. It was approved in most European countries in 1990, approved in the United States in 1992, and included in the United States Pharmacopoeia. Some compani...

Claims

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Application Information

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IPC IPC(8): C07H1/00C07H17/08
CPCC07H1/00C07H17/08
Inventor 袁庆叶海波王法平
Owner ZHEJIANG KANGMU PHARMA
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