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Process for preparing cefquinome sulfate

A technology of cefquinome sulfate and aminocefotaxime, which is applied in the field of preparation of cefquinome sulfate, can solve problems such as high production cost and unstable quality of cefotaxime acid, and achieve product quality improvement, good therapeutic effect, and responsiveness The effect of mild conditions

Inactive Publication Date: 2008-11-19
崔增学
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But the quality of cefotaxime acid is not stable at present, so the production cost is relatively high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] One, the preparation of 7-aminocefaquine

[0022] Under nitrogen protection, put 100ml of dichloromethane into a 250ml dry four-neck flask, cool to 0°C, add 9ml (0.0625mol) iodotrimethylsilane, keep it below 0°C and add 9ml (0.076mol) of 5 dropwise, 6,7,8-tetrahydroquinoline, stirred for 30 minutes after dropping. Add 3.4g (0.0125mol) 7-ACA, heat up to reflux for 2h, and cool to 5°C. Add 100mlC dropwise 2 h 5 OH / H 2 O=7:1 (volume ratio) mixed solvent, stirred for 4h. After suction filtration, the filter cake was washed with 50 ml of cold dichloromethane and 50 ml of cold acetone, and dried in vacuo to obtain 4.97 g of light yellow crystals with a yield of 81.0%.

[0023] Two, cefquinome sulfate preparation

[0024] Put 40ml tetrahydrofuran and 20ml water into a 100ml three-neck flask, add 2.45g (0.005mol) 7-ACQ, add sulfuric acid dropwise until 7-ACQ dissolves, add activated carbon and stir for 30 minutes to decolorize. Suction filtration, cooling the filtrate to...

Embodiment 2

[0026] One, the preparation of 7-aminocefaquine

[0027] Under nitrogen protection, put 80ml of dichloromethane into a 250ml dry four-necked flask, cool to 0°C, add 9ml (0.0625mol) iodotrimethylsilane, keep it below 5°C and add dropwise 8.5ml (0.072mol) of 5 , 6,7,8-tetrahydroquinoline, stirred for 30min after the drop was completed. Add 3.4g (0.0125mol) 7-ACA, heat up to reflux for 2h, and cool to 5°C. Add 100mlC dropwise 2 h 5 OH / H 2 O=5:1 (volume ratio) mixed solvent, stirred for 4h. After suction filtration, the filter cake was washed with 50 ml of cold dichloromethane and 50 ml of cold acetone, and dried in vacuo to obtain 4.88 g of light yellow crystals with a yield of 79.5%.

[0028] Two, cefquinome sulfate preparation

[0029] Put 40ml tetrahydrofuran and 20ml water into a 100ml three-neck flask, add 2.45g (0.005mol) 7-ACQ, add sulfuric acid dropwise until 7-ACQ dissolves, add activated carbon and stir for 30 minutes to decolorize. Filtrate with suction, cool th...

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Abstract

The invention discloses a method for preparing cefquinome sulfate, belonging to the cephalosporin antibiotics special for animals. The method comprises the following: A. a step of preparing 7-amino-cefquinome, during which, iodotrimethylsilane reacts with 5, 6, 7, 8-tetrahydroquinoline, and a reaction product reacts with 7-amino-cephalosporanic acid, thereby obtaining the 7-amino-cefquinome; B. a step of preparing the cefquinome sulfate, during which, the 7-amino-cefquinome reacts with AE active ester after the 7-amino-cefquinome is dissolved and is decolored by sulphuric acid, and the cefquinome sulfate is obtained after the reaction product is subject to extraction, suction filtering, leaching and drying. The method uses 7-ACA which is widely used in industry, is low in cost and is easily obtained as a raw material, without using cefotaxime acid with unstable service quality; meanwhile, the method has a mild reaction condition and simple operation, reduces the dosage of the 5, 6, 7, 8-tetrahydroquinoline which is an important intermediate, and greatly improves the product quality with the yield of 64.1 percent and the purity of 99.7 percent, thereby the method is suitable for industrial production.

Description

technical field [0001] The present invention relates to a kind of preparation method of animal special medicine, specifically, the present invention is a kind of preparation method of cefquinome sulfate. Background technique [0002] At present, cephalosporin antibiotics, as a new type of special antibiotics, have the advantages of broad spectrum, high efficiency, low toxicity and low residue, and can be directly used in animal health care. Chinese patent application No. 200610048424.0 (published on January 23, 2008) discloses a method for preparing cefquinol sulfate. In the method, cefotaxime acid is used as a raw material to react with tetrahydroquinoline to obtain the cefquinol product, which is then extracted, decolorized by active carbon, reacted with sulfuric acid in an ethanol solution to obtain the final product cefquinol sulfate. However, the quality of cefotaxime acid is not stable at present, so the production cost is relatively high. Contents of the invention ...

Claims

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Application Information

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IPC IPC(8): C07D501/46A61P31/04
Inventor 李长青崔增学
Owner 崔增学
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