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Preparation method of diterpene-based antibiotic for livestock and poultry

A technology for generating formulas and compounds, which is applied in the field of preparation of diterpene-based antibiotics for livestock and poultry, can solve problems such as the impact of industrial production of compounds and the reduction in the conversion rate of target products, and achieve stable properties, less impurities, and simple preparation processes Effect

Active Publication Date: 2019-02-26
保定加合精细化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But, because diethylaminoethanethiol is particularly easily oxidized during the reaction, the conversion rate of the target product is reduced, which has an adverse effect on the industrial production of the compound shown in formula I

Method used

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  • Preparation method of diterpene-based antibiotic for livestock and poultry
  • Preparation method of diterpene-based antibiotic for livestock and poultry
  • Preparation method of diterpene-based antibiotic for livestock and poultry

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Add 120mL of toluene and 60mL of water into a 500mL three-necked flask, then add 14.16g (0.062mol) of diethylaminoethylthiobenzoate, 2.604g of lithium hydroxide monohydrate, and 3.22g of tetrabutylammonium hydroxide, stir for 30min, and slowly 30 g (0.062 mol) of pleuromutilin benzoate was added, and after the addition was complete, the temperature was raised to 75°C-80°C, and the reaction was kept for 6 hours, and the reaction was completed. The sample was quantified by HPLC, and 29.91 g of the compound represented by formula I was obtained, with a conversion rate of 94.6%. HPLC purity 98.5558%, see the spectrum and data Figure 4 and 5 .

Embodiment 2

[0043] Add 120mL of toluene and 60mL of water into a 500mL three-necked flask, then add 18.67g (0.062mol) of diethylaminoethylthio p-toluenesulfonate, 6.25g of liquid caustic soda (NaOH), 0.25g of tetrabutylammonium chloride, and stir for 20min , slowly added 30 g (0.062 mol) of pleuromutilin benzoate, after the addition was complete, the temperature was raised to 80° C.-85° C., and the reaction was kept for 7.5 hours, and the reaction was completed. The sample was quantified by HPLC, and the compound represented by formula I was obtained, and the conversion rate was 93.6%. HPLC purity 98.8715%.

Embodiment 3

[0045] Add 120mL of toluene and 60mL of water into a 500mL three-necked flask, then add 18.36g (0.062mol) of diethylaminoethylthio-p-nitrobenzoate and 6.25g of liquid caustic soda, stir for 10min, and slowly add pleuromutilin benzoic acid 30 g (0.062 mol) of ester, after the feeding is completed, the temperature is raised to 75°C-85°C, and the reaction is kept for 6.5 hours, and the reaction is completed. Sampling was carried out by HPLC for quantification, and 29.66 g of the compound represented by formula I was obtained, with a conversion rate of 93.8%. HPLC purity 99.1115%.

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Abstract

The invention provides a preparation method of a diterpene-based antibiotic for livestock and poultry. According to the present invention, with the preparation method, the disadvantage that diethylaminoethanethiol used by the process in the prior art is easily oxidized during the reaction is avoided; and the experimental results show that the reaction raw materials are stable during the reaction,the diterpene-based antibiotic for livestock and poultry can be generated by the reaction at the high conversion rate, the by-product of the reaction is less, the single impurity is less, and the preparation process is simple, and meets the requirements of industrial production.

Description

technical field [0001] The invention belongs to the field of veterinary drugs, and relates to a preparation method of diterpene antibiotics for livestock and poultry. Background technique [0002] The compound represented by formula I (CAS No. 55297-95-5) is a diterpene antibiotic for poultry and poultry used for preventing and treating poultry respiratory diseases and promoting animal growth. [0003] [0004] Currently, the prior art uses diethylaminoethanethiol as an important intermediate for the production of compounds represented by formula I. However, since diethylaminoethanethiol is particularly easily oxidized during the reaction process, the conversion rate of the target product is reduced, which adversely affects the industrial production of the compound shown in formula I. [0005] Therefore, it is necessary to find a new method for preparing the compound shown in formula I. Contents of the invention [0006] Aiming at the above-mentioned shortcomings and ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C323/52C07C319/14
CPCC07C319/14C07C323/52Y02A40/70
Inventor 王永杰章先江
Owner 保定加合精细化工有限公司
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