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Recovery method of piperazine in condensation mother liquor for preparing ciprofloxacin

The technology of a ciprofloxacin and a recovery method, which is applied in directions such as organic chemistry, can solve problems such as the excessive cost ratio of piperazine products, and achieve the effects of low production cost, improved economic benefit and convenient operation.

Active Publication Date: 2014-04-30
ZHEJIANG LANGHUA PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] For the above-mentioned problems that exist in the prior art, the object of the present invention is to provide a kind of recovery method of piperazine in the condensation mother liquor that prepares ciprofloxacin, and overcome the problem that piperazine is too high in the product cost, have solved The recovery problem of piperazine

Method used

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  • Recovery method of piperazine in condensation mother liquor for preparing ciprofloxacin
  • Recovery method of piperazine in condensation mother liquor for preparing ciprofloxacin

Examples

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Effect test

Embodiment 1

[0020] Example 1 Concentrate the condensation mother liquor obtained in the embodiment of the preparation of the ciprofloxacin-piperazine condensation mother liquor to remove most of the water, so that the piperazine content is 20-40%, dissociate to PH11 with solid NaOH, and determine by acid-base potentiometric titration The piperazine content is 28.2%, so 20g of the piperazine condensation mother liquor with a piperazine content of 28.2% contains 5.64g of piperazine. Take the above 20g Piperazine condensation mother liquor with a piperazine content of 28.2%, at 20°C, add 40g 30% KF aqueous solution, a large amount of solids were precipitated, kept stirring for 30 minutes, and suction filtered to obtain a wet weight of 12.6g piperazine hexahydrate solid, 44.8g filtrate, the piperazine content of the filtrate was 1.7%, and the piperazine recovery rate was 86.5%.

Embodiment 2

[0021] Example 2 At 25°C, add the free 20g piperazine condensation mother liquor with a piperazine content of 28.2% obtained in Example 1 40g 40% KF aqueous solution, a large number of solids were precipitated, kept stirring for 50 minutes, and suction filtered to obtain a wet weight of 14.2g piperazine hexahydrate solid, 44g filtrate, the piperazine content of the filtrate was 0%, and the piperazine recovery rate was 100%.

Embodiment 3

[0022] Example 3 At 30°C, the free 20g piperazine condensation mother liquor with a piperazine content of 28.2% obtained in Example 1 was added 40g 50% KF aqueous solution, a large number of solids were precipitated, kept stirring for 20 minutes, and suction filtered to obtain a wet weight of 11g of piperazine hexahydrate solid, and 47g of filtrate. The piperazine content of the filtrate was 0%, and the recovery rate of piperazine was 100%.

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Abstract

The invention provides a recovery method of piperazine in condensation mother liquor for preparing ciprofloxacin, belonging to the technical field of fine chemical engineering. The recovery method comprises the following steps of: removing most water from condensation mother liquor for preparing ciprofloxacin, adjusting PH to be 11-14 by inorganic base, cooling to 20-30 DEG C, adding potassium fluoride water solution to separate out solid, stirring for 20-50min by means of heat preservation, and filtering to obtain the piperazine. According to the recovery method, the condensation mother liquor for preparing the ciprofloxacin is evaporated to dryness in a concentrating way, and is ionized by the inorganic base, so that the concentrated residue can be dissolved, therefore, the detection accuracy of the piperazine content can be conveniently guaranteed by an acid-base potentiometric titration method, and the recovery conveniences of the piperazine can be preferably guaranteed; and the recovery method of the invention is simple in technology, and short in time, the yield can be more than 86.6%, the recovery method is low in production cost, simple to operate, free of toxicity and environment-friendly, and the economic benefit can be greatly improved, so that the recovery method is suitable for large-scale industrial production.

Description

technical field [0001] The invention belongs to the technical field of fine chemicals, and in particular relates to a method for recovering piperazine in condensation mother liquor for preparing ciprofloxacin with simple operation and high recovery rate. Background technique [0002] Ciprofloxacin, the chemical name is 1-cyclopropyl-6-fluoro-1,4-dihydro-4-oxo-7-(1-piperazinyl)-3-quinolinecarboxylic acid (formula (i )), is the third generation of quinolone antibacterial drugs. It was successfully synthesized by Bayer Pharmaceuticals in Germany in 1981, and its structure is as follows: [0003] [0004] At present, ciprofloxacin is mainly obtained from ciprofloxacin intermediate 1-cyclopropyl-6-fluoro-7-chloro-1,4-dihydro-4-oxo-3-quinolinecarboxylic acid (formula (ii) ) The initial synthesis process has been basically mature, and most of them use piperazine (formula (iii)) for autocatalytic reaction. The response is as follows: [0005] [0006] In the existing proce...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D295/023C07D295/027
Inventor 林邦平杜晓东王忠美黄明孙
Owner ZHEJIANG LANGHUA PHARMA