Recovery method of cefprozil

A technology of cefprozil and recovery method, which is applied in the direction of organic chemistry, can solve the problems of environmental pollution, waste of resources, etc., and achieve the effects of convenient operation, reduced pressure, and simple process

Inactive Publication Date: 2013-02-06
南通康鑫药业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Generally, a certain amount of cefprozil remains in the cefprozil mother liquor after synthesis and extraction. If ...

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0010] At 25°C, put in 500g of cefprozil refined mother liquor, stir and lower the temperature to -5°C, then add 803g of dimethylformamide and 104g of acetone dropwise at -7°C, after dropping, stir for 5h, filter with 200ml Wash with acetone, drain, and dry under vacuum at 30°C to obtain 12.6 g of crude cefprozil;

[0011] Add the above dried crude product into 28.7g of purified water and 53.2g of isopropanol mixed solvent, adjust the pH to 1.2 with 15% hydrochloric acid, stir at 20-30°C for 30min, add 0.6g of activated carbon, and decolorize at 28°C for 45min , filter with suction, wash the activated carbon with 20ml of purified water, combine with the filtrate, adjust the pH to 6.5-6.6 with concentrated ammonia water at a temperature of 26°C, stir for 60 minutes, cool down to 5°C, stir for 30 minutes at a temperature of 0-5°C, and filter with suction. Finally, it was washed with 80ml of acetone, drained, and vacuum-dried at 30°C for 4 hours to obtain 9.28g of cefprozil finis...

Embodiment 2

[0013] At 23°C, put in 500g of cefprozil refined mother liquor, stir and cool down to -5°C, then add 803g of dimethylformamide and 104g of acetone dropwise at -9°C, after dropping, stir for 5h, filter with 200ml Washed with acetone, drained, and dried under vacuum at 30°C to obtain 13.1 g of crude cefprozil;

[0014] Add the above-mentioned dried crude product into 29.6g of purified water and 55.9g of isopropanol mixed solvent, adjust the pH to 1.3 with 15% hydrochloric acid, stir at 20-30°C for 30min, add 0.6g of activated carbon, and decolorize at 28°C for 45min , filter with suction, wash the activated carbon with 20ml of purified water, combine with the filtrate, adjust the pH to 6.5-6.6 with concentrated ammonia water at a temperature of 26°C, stir for 60 minutes, cool down to 5°C, stir for 30 minutes at a temperature of 0-5°C, and filter with suction. Finally, it was washed with 80ml of acetone, drained, and vacuum-dried at 30°C for 4 hours to obtain 9.36g of cefprozil f...

Embodiment 3

[0016] At 27°C, put in 500g of cefprozil refined mother liquor, stir and cool down to -5°C, add 803g of dimethylformamide and 104g of acetone dropwise at -6°C, after the dripping is complete, stir for 5.5h, filter with suction, Washed with 200ml of acetone, drained, and vacuum-dried at 30°C to obtain 12.9g of cefprozil crude product;

[0017] Add the above dried crude product into 26.7g of purified water and 53.4g of isopropanol mixed solvent, adjust the pH to 1.1 with 15% hydrochloric acid, stir at 20-30°C for 30min, add 0.6g of activated carbon, and decolorize at 28°C for 45min , filter with suction, wash the activated carbon with 20ml of purified water, combine with the filtrate, adjust the pH to 6.5-6.6 with concentrated ammonia water at a temperature of 26°C, stir for 60 minutes, cool down to 5°C, stir for 30 minutes at a temperature of 0-5°C, and filter with suction. Finally, it was washed with 80ml of acetone, drained, and vacuum-dried at 30°C for 4 hours to obtain 9.31...

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PUM

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Abstract

The invention discloses a recovery method of cefprozil. The method comprises the steps of dripping dimethylformamide and acetone in a cefprozil refined mother solution to obtain the crude cefprozil; adding the crude cefprozil into a mixed solvent, adjusting the pH value of the solution with hydrochloric acid, activated carbon fading, and adjusting the pH value of stronger ammonia water; and finally cooling crystallization, suction filtration and drying to obtain the end product of cefprozil. The recovery method has the advantages that 95% of cefprozil can be extracted from the mother solution, so that the wastewater treatment pressure is greatly reduced, and the end product meets the pharmacopeia standards after recovery and treatment; and in addition, the recovery method is simple and convenient to operate, and dimethylformamide, acetone and isopropanol can be recycled and utilized.

Description

technical field [0001] The invention relates to a method for recovering cefprozil. Background technique [0002] Cefprozil is a second-generation non-ester oral cephalosporin developed by Bristol-Myers Tokyo Research Institute in 1983. Its chemical name is (6R,7R)-7-[(2R)-amino-(4-hydroxyphenyl )Acetamido]-8-oxidation-3-(1-propenyl)-5-thio-1-azabicyclo[4.2.0]oct-2-ene-2-carboxylic acid, this product is harmful to leather Both blue-positive and negative bacteria have strong antibacterial activity, which can inhibit the synthesis of bacterial cell walls and make the bacteria rapidly rupture and dissolve. Generally, a certain amount of cefprozil remains in the cefprozil mother liquor after synthesis and extraction. If it is directly discharged with waste water, it will not only pollute the environment, but also cause waste of resources. Contents of the invention [0003] The purpose of this invention is to provide a kind of recovery method of cefprozil. [0004] In order t...

Claims

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Application Information

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IPC IPC(8): C07D501/22C07D501/12
Inventor 唐子安
Owner 南通康鑫药业有限公司
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