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,

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0023] Method for preparing hydrochloride cefur, including the steps of:

[0024] Step 1, preparation of cefuroofur

[0025] The 7-ACF was added to the organic solvent, and the alkaline is added dropwise, then the AE active ester, the insulation reaction, and the reaction is completed, and the hydrochloride cefiofur is filtered.

[0026] Step 2, refined hydrochloride cefiururo

[0027] Add the steps of hydrochloride, cefuroyofur, add the alkali, and add the alkali to filter, then add hydrochloride filtration, adding the hydrochloric acid pH, filtrate, adding organic solvent, crystallization, filtration, drying, to obtain a white product, ie is hydrochloric acid Ceforezola.

[0028] Further, step one, after the reaction is completed, the hydrochloric acid is adj to <1.0.

[0029] Further, the mass ratio of water using water in step II is 1 to 3 using the mass ratio of 7-ACF in the step one.

[0030] Further, in step two, the base includes one or more of sodium hydroxide, sodium bic...

Example Embodiment

[0035] Example 1

[0036] Acetone was added to the reaction flask, and 20 g of 7-ACF was added, and the mixture was added dropwise to dissolution. AE active ester was added, and the reaction was added 3-4 h. After completion of the reaction, pH <1.0, cooling crystallization, filtration, to give the cefosporozoexide.

[0037] The cefuroyofura was added to the reaction bottle, add 40 g of water, stirred, dripped with sodium carbonate solution, tensile pH to 8.5, stirred, and activated carbon 2 g, stirred for 0.5 h, filtration. The filtrate was added dropwise pH <1.0, and acetone was continued to 120 mL, crystallized crystals crystalline, filtered, filter, filter, dried, dried to give a white crystalline phrolene cefothoiofuride 29.8 g, and content 99.3%.

Example Embodiment

[0038] Example 2

[0039] Acetonitrile was added to the reaction flask, and 20 g7-ACF was added, and the mixture was added dropwise to dissolution. AE active ester was added, and at 15 ° C for 3-4 h. After completion of the reaction, pH <1.0, cooling crystallization, filtration, to give the cefosporozoexide.

[0040] The hydrochloride cefurolazo was added to the reaction bottle, add 30 g of water, stirred, and triethylamine was added dropwise, and pH to 9.0, stirred, and activated carbon 2 g, stirred for 0.5 h, filtered. The filtrate was added dropwise pH <1.0, and the acetonitrile was added dropwise to 100 mL, crystallized crystals crystalline, filtered, filter, filter, dried, dried to give a white crystalline phrolene phroiofuride 30.0 g, and the content was 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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