Preparation method of ceftiofur hydrochloride

A technology of ceftiofur hydrochloride and hydrochloric acid, which is applied in the field of preparation of ceftiofur hydrochloride, can solve the problems of large amount of acetone, low extraction efficiency, and large amount of waste water, and achieve high product purity and yield, high yield, and high dosage little effect

Pending Publication Date: 2022-03-29
河南立诺制药有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the method disclosed in patent CN102993216A, after the reaction, the reaction solution is extracted with water, the extraction efficiency is low, and there is a lot of waste water. The wet product of ceftiofur hydrochloride is dissolved with 10 times acetone, and the amount of acetone is large

Method used

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preparation example Construction

[0023] A preparation method of ceftiofur hydrochloride, comprising the steps of:

[0024] Step 1, preparation of ceftiofur hydrochloride crude product

[0025] Add 7-ACF into the organic solvent, add organic base dropwise to dissolve the clear, then add AE active ester, keep warm for reaction, after the reaction, add hydrochloric acid to adjust the pH, filter to obtain the crude product of ceftiofur hydrochloride;

[0026] Step 2, refining ceftiofur hydrochloride

[0027] Add the crude ceftiofur hydrochloride obtained in step 1 into water, add alkali to adjust the pH to dissolve, then add activated carbon to filter, add hydrochloric acid to adjust the pH, add an organic solvent to the filtrate dropwise, crystallize, filter, and dry to obtain a white product, which is hydrochloric acid Ceftiofur.

[0028] Further, in step 1, after the reaction is completed, hydrochloric acid is added to adjust the pH to <1.0.

[0029] Further, the mass ratio of water used in step 2 to 7-ACF ...

Embodiment 1

[0036] Add acetone to the reaction flask, put 20g of 7-ACF into it, add organic base dropwise and stir until dissolved. Add AE active ester and react for 3-4h. After the reaction, add hydrochloric acid to adjust the pH<1.0, cool down to crystallize, and filter to obtain crude ceftiofur hydrochloride.

[0037] Add crude ceftiofur hydrochloride to the reaction flask, add 40 g of water, stir, add dropwise sodium carbonate solution, adjust the pH to 8.5, stir to dissolve, add 2 g of activated carbon, stir for 0.5 h, and filter. The filtrate was added dropwise with hydrochloric acid to adjust the pH to <1.0, and continued to add dropwise acetone to 120ml. After crystallization, the temperature was lowered to crystallize, filtered, the filter cake was rinsed with water, drained, and dried to obtain 29.8g of white crystalline ceftiofur hydrochloride with a content of 99.3%.

Embodiment 2

[0039] Add acetonitrile into the reaction flask, put 20g of 7-ACF into it, add organic base dropwise and stir until dissolved. Add AE active ester and react at 15°C for 3-4h. After the reaction, add hydrochloric acid to adjust the pH<1.0, cool down to crystallize, and filter to obtain crude ceftiofur hydrochloride.

[0040] Add crude ceftiofur hydrochloride to the reaction flask, add 30g of water, stir, add triethylamine dropwise, adjust the pH to 9.0, stir to dissolve, add 2g of activated carbon, stir for 0.5h, and filter. Add hydrochloric acid dropwise to the filtrate to adjust pH<1.0, continue to add acetonitrile dropwise to 100ml, cool down to crystallize after crystallization, filter, rinse the filter cake with water, drain, and dry to obtain 30.0g of white crystalline ceftiofur hydrochloride with a content of 99.2%.

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PUM

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Abstract

The invention provides a preparation method of ceftiofur hydrochloride, which comprises the following steps: step 1, preparation of a ceftiofur hydrochloride crude product: adding 7-ACF into an organic solvent, dropwise adding organic alkali for dissolving, then adding AE active ester, carrying out heat preservation reaction, after the reaction is finished, adding hydrochloric acid to adjust the pH, and filtering to obtain the ceftiofur hydrochloride crude product; and 2, refining the ceftiofur hydrochloride, adding the crude ceftiofur hydrochloride product obtained in the step 1 into water, adding alkali to adjust the pH value, dissolving, filtering by adding activated carbon, adding hydrochloric acid to adjust the pH value, dropwise adding an organic solvent into the filtrate, crystallizing, filtering and drying to obtain a white product, namely the ceftiofur hydrochloride. In the preparation process, the solvent amount is small, the solvent can be recycled and reused, waste water is little, the method is more environmentally friendly, the purity of the product ceftiofur hydrochloride reaches 99.0% or above, the reaction yield is high, and the appearance color is good; the method is simple in preparation process, short in production period, high in product purity, high in yield, economical and environment-friendly.

Description

technical field [0001] The invention relates to the technical field of preparation of ceftiofur hydrochloride, in particular to a preparation method of ceftiofur hydrochloride. Background technique [0002] Ceftiofur is the first third-generation cephalosporin antibiotic specially used for animals. It was successfully developed by Pharmacia-Upjohn and marketed as its sodium salt lyophilized powder and hydrochloride suspension. 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 diseases such as cattle, sheep, pigs, dogs, and chickens all over the world. [0003] Ceftiofur hydrochloride is the hydrochloride salt of ceftiofur, which is relatively stable and can be valid for more than two years. Its oil suspension injection can be used for hoof disease, infection, and 3-shot health care for piglets, etc., with good results. [0004] U.S. Patent 68...

Claims

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Application Information

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IPC IPC(8): C07D501/06C07D501/12C07D501/36
CPCC07D501/12C07D501/36C07D501/06
Inventor 唐红岩张杰
Owner 河南立诺制药有限公司
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