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Method for preparing tulathromycin

A teramycin and reactor technology, which is applied in the field of preparing teramycin, can solve the problems of large amount of n-propylamine, low content of crude product, bad properties, etc., and achieves the effects of improved selectivity and good quality of crude product

Inactive Publication Date: 2016-06-08
杭州海尔希畜牧科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The present invention provides a method for preparing telamycin, which mainly solves the problem of the large amount of n-propylamine used in the prior art; Not good, need to form a technical problem of phosphate re-neutralization and purification

Method used

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  • Method for preparing tulathromycin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Embodiment 1: a kind of method for preparing telamycin of this example, its steps are:

[0023] a. Add epoxy intermediate (III) (747g, 1.0mol), isopropanol (5950g), N-benzylpropylamine (178.8g, 1.2mol) to the reactor and stir well, then heat to 50-60 ℃ stirring reaction for 36 hours;

[0024] b. After completion of the reaction, concentrate and remove most of the solvent, then add acetone (7450g), stir and transfer to the pressure reactor;

[0025] c. Add 10% palladium-carbon catalyst (74.7g) in the pressure reactor, feed hydrogen, keep the reaction solution at 20-30°C, stir and react under 50psi pressure for 24 hours, filter and recover the catalyst after the reaction, and concentrate to remove most of it Solvent, then water (7470g) was added, the precipitated solid was collected by filtration, and the crude product of telamycin was obtained after vacuum drying. After recrystallization, 621.7g of fine product was obtained, with a yield of about 77.1%.

[0026] The co...

Embodiment 2

[0027] Embodiment 2: a kind of method for preparing telamycin of this example, its steps are:

[0028] a. Add epoxy intermediate (III) (747g, 1.0mol), isopropanol (3750g), N-benzylpropylamine (149g, 1.0mol) into the reactor and stir well, then heat to 50-60°C Stir the reaction for 24 hours;

[0029] b. After completion of the reaction, concentrate and remove most of the solvent, then add acetone (6000g), stir and transfer to the pressure reactor;

[0030] c. Add 10% palladium-carbon catalyst (74.7g) in the pressure reactor, feed hydrogen, keep the reaction solution at 20-30°C, stir and react under 50psi pressure for 20 hours, filter and recover the catalyst after the reaction, and concentrate to remove most of it Solvent, and then add water (7470g), filter and collect the precipitated solid, obtain the crude product of telamycin after vacuum drying, obtain the fine product 435.6g after recrystallization, the yield is about 54.0%.

[0031] The content of the obtained fine tel...

Embodiment 3

[0032] Embodiment 3: a kind of method for preparing telamycin of this example, its steps are:

[0033] a. Add epoxy intermediate (III) (747g, 1.0mol), isopropanol (4800g), N-benzylpropylamine (163.9g, 1.1mol) to the reactor and stir well, then heat to 50-60 ℃ stirring reaction for 30 hours;

[0034] b. After completion of the reaction, concentrate and remove most of the solvent, then add acetone (6700g), stir and transfer to the pressure reactor;

[0035] c. Add 10% palladium-carbon catalyst (74.7g) in the pressure reactor, feed hydrogen, keep the reaction solution at 20-30°C, stir and react under 50psi pressure for 22 hours, filter and recover the catalyst after the reaction, and concentrate to remove most Solvent, then add water (7470g), filter and collect the precipitated solid, obtain the crude product of telamycin after vacuum drying, and obtain 503.8g of fine product after recrystallization, the yield is about 62.5%.

[0036] The content of the obtained fine telamycin ...

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Abstract

The invention relates to large-loop type veterinary medicine antibiotics, in particular to a method for preparing tulathromycin. The method mainly solves the problem that in the prior art, the dosage of n-propylamine is large, and also solves the technical problems that due to the large dosage of n-propylamine, a crude product is not high in content and poor in character, and phosphate needs to be formed, neutralized and purified. The method comprises the steps that an epoxy intermediate, ethyl alcohol or isopropanol and N-benzyl propylamine are added into a reactor and stirred fully and evenly, and then heating and stirring are carried out for a reaction; after the reaction is finished, a solvent is removed, acetone is added, and the mixture is evenly stirred and then transferred into a pressure reactor; a palladium carbon catalyst is added in the pressure reactor, hydrogen is introduced, a reaction is carried out under stirring, the catalyst is recycled through filtering after the reaction is finished, concentration is carried out to remove the solvent, then water is added, filtering is carried out, separated-out solids are collected and subjected to vacuum drying, a tulathromycin crude product is obtained, and a fine tulathromycin product is obtained after recrystallization.

Description

technical field [0001] The invention relates to a macrocyclic veterinary drug antibiotic, in particular to a method for preparing telamycin. Background technique [0002] In recent years, Tyramycin, as an important macrocyclic veterinary antibiotic, can be used as an antibacterial and antiprotozoal agent for mammals, fish and birds, and its market acceptance and usage rate have increased significantly in recent years. [0003] Tyramycin is mainly produced and sold by U.S. Pfizer at present, and its main production method has also applied for a corresponding patent (CN1297564). In this method, n-propylamine is directly used as a ring-opener after it has prepared an epoxy intermediate, and the reaction The crude product of telamycin is obtained, and neutralized and purified after forming phosphate to obtain the refined product of telamycin. [0004] The product prepared by the method has better appearance and shape and higher content. However, in order not to form a disubsti...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H17/00C07H1/00
CPCY02P20/584C07H17/00C07H1/00
Inventor 楼伟杰徐求文蒋忠良曹爱玲
Owner 杭州海尔希畜牧科技有限公司
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