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Recovery method of cefprozil
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A technology of cefprozil and recovery method, which is applied in the direction of organic chemistry, etc., to achieve the effects of reducing pressure, convenient operation and simple process
Inactive Publication Date: 2015-03-11
南通康鑫药业有限公司
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Abstract
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Problems solved by technology
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 a waste of resources.
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Embodiment 1
[0013] At 23°C, put 500g of cefprozil mother liquor after synthesis and extraction, 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, and filter with suction , washed with 200ml of acetone, drained, and vacuum-dried at 30°C to obtain 13.1g of cefprozil crude product;
[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 ...
Embodiment 2
[0016] At 27°C, put 500g of cefprozil mother liquor after synthesis and extraction into it, stir and cool down to -5°C, then add 803g of dimethylformamide and 104g of acetone dropwise at -6°C, after dropping, stir for 5.5h, pump Filtered, washed with 200ml of acetone, sucked dry, and dried under vacuum 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 ...
Embodiment 3
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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 carbonfading, 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 ord...
Claims
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