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Preparation method of ceftiofur intermediate

A technology of ceftiofur and its intermediates, which is applied in the field of preparation of compound intermediates, can solve the problems of difficulty in synthesis and quality control, and achieve the effects of convenient product quality, fast reaction progress, and high purity

Inactive Publication Date: 2019-03-05
王小桥
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There are few reports on the synthesis of this drug, and there are certain difficulties in synthesis and quality control

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] (1) Weigh 36g of sodium hydrosulfide and dissolve it in 4 times of water, stir to dissolve at 25°C, slowly add furoyl chloride dropwise, after the dropwise addition, stir for 20 minutes, add ethyl acetate equal to the volume of water, adjust the pH value to 1.0 with hydrochloric acid , stand for stratification, remove the water phase; add 4 times of water, adjust the pH=10 with sodium hydroxide solution, stand for stratification, remove the organic phase, add new ethyl acetate, adjust the pH value=3.0 with hydrochloric acid, static Separate the layers, remove the water phase, dry the organic phase with anhydrous magnesium sulfate, filter, and save the filtrate;

[0014] (2) Measure 40ml of ethyl acetate into the reaction bottle, add boron trifluoride etherate complex, start stirring, cool down, add the dried filtrate, add 20g of 7-ACA, stir for 10 minutes, control the temperature at 35°C, and keep warm After reacting for 2 hours, cool down to 0-5°C, add 100ml of ice wat...

Embodiment 2

[0016] (1) Weigh 36g of sodium hydrosulfide and dissolve it in 4 times of water, stir to dissolve at 25°C, slowly add furoyl chloride dropwise, after the dropwise addition, stir for 20 minutes, add ethyl acetate equal to the volume of water, adjust the pH value to 1.0 with hydrochloric acid , stand for stratification, remove the water phase; add 4 times of water, adjust the pH=8 with sodium bicarbonate solution, stand for stratification, remove the organic phase, add new ethyl acetate, adjust the pH value to 1.0 with hydrochloric acid, and statically Separate the layers, remove the water phase, dry the organic phase with anhydrous magnesium sulfate, filter, and save the filtrate;

[0017] (2) Measure 40ml of ethyl acetate into the reaction bottle, add boron trifluoride etherate complex, start stirring, cool down, add the dried filtrate, add 20g of 7-ACA, stir for 10 minutes, control the temperature at 35°C, and keep warm After reacting for 2 hours, cool down to 0-5°C, add 100m...

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PUM

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Abstract

The invention discloses a preparation method of a ceftiofur intermediate. The method comprises the steps of taking 2-furoyl chloride as a raw material to react with sodium hydrosulfide, extracting impurities by ethyl acetate twice to obtain a higher-purity ethyl acetate solution of thiofuroic acid, and adding 7-ACA for condensation to obtain the ceftiofur intermediate. In the present invention, the pH is adjusted by using an alkali solution, first extraction is carried out by using ethyl acetate, then the pH value is adjusted with an acid solution, and second extraction is carried out by usingethyl acetate, thereby achieving the effect of removing impurities, and more facilitating reaction with 7-ACA. After the purification step is added, the appearance and quality of the obtained intermediate product are significantly improved, and when the ceftiofur intermediate is used for synthesis of ceftiofur, the yield and quality are obviously improved.

Description

technical field [0001] The invention relates to a preparation method of a compound intermediate, in particular to a preparation method of a ceftiofur intermediate. Background technique [0002] Ceftiofur is the first third-generation cephalosporin antibiotic exclusively for animals, successfully developed by Pharmacia-Upjohn. Because of its strong antibacterial activity, excellent pharmacokinetic characteristics, small toxic and side effects, and low residue, it is widely used in the treatment of bacterial respiratory tract infections in livestock all over the world. There are few reports on the synthesis of this drug, and there are certain difficulties in synthesis and quality control. Contents of the invention [0003] The purpose of the present invention is to provide a preparation method of a ceftiofur intermediate. After adding purification steps, the appearance and quality of the intermediate product are significantly improved. When used in the synthesis of ceftiofu...

Claims

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Application Information

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IPC IPC(8): C07D501/18C07D501/04
CPCC07D501/18C07D501/04
Inventor 王小桥王存亮伍重远熊玲玲
Owner 王小桥