Cefprozil mother liquor application technique

A technology of cefprozil and propylene mother liquor, which is applied in the field of medicine, can solve problems such as large solvent consumption and energy consumption, and product quality does not meet the requirements, and achieves significant economic and environmental benefits, convenient operation, and simple mother liquor application process

Active Publication Date: 2018-10-16
TOPFOND PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] Chinese patent CN102911187A, after cooling the refined mother liquor of cefprozil, add dimethylformamide and acetone to process, obtain cefprozil dimethylformamide solvate, and o

Method used

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  • Cefprozil mother liquor application technique

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Take 28.4g of 7-APRA (cephalosporin core), add 200mL of dichloromethane, 15g of hexamethyldisilazane, 9.8g of trimethylchlorosilane and 1g of imidazole to three-necked flask A, and heat to reflux for 3h ;

[0038] Take 91.2g of p-hydroxyphenylglycine Deng potassium salt, add 200mL of dichloromethane and 150mL of DMF (dimethylformamide) in a three-necked flask B, drop the temperature to -50℃ and add ethyl chloroformate dropwise, control the temperature -33℃- React at 43℃ for 3h;

[0039] After the reaction, the active ester in the three-necked flask B was cooled to below -50°C, and the medium protective group mixture in the three-necked flask A was added dropwise. The temperature was controlled at -50°C and reacted for 2 hours to obtain cefprozil. Add 110mL crude cefprozil refined mother liquor and 9mL saturated FeCl to the reaction solution 3 The solution, add hydrochloric acid to adjust the pH value to 1.0, raise the temperature to 5℃-8℃, stir for 30min under temperature c...

Embodiment 2

[0042] Take 28.4g of 7-APRA, add 200mL of dichloromethane, 15.5g of hexamethyldisilazane, 9.8g of trimethylchlorosilane and 1g of imidazole to the three-neck flask A, and heat to reflux for 3h;

[0043] Take 91.2g of p-hydroxyphenylglycine Deng potassium salt, add 200mL of dichloromethane and 150mL of DMF to a three-necked flask B, drop the temperature to -50℃, add ethyl chloroformate, and control the temperature to -33℃-43℃ for 3h;

[0044] After the reaction, the active ester in the three-necked flask B was cooled to below -50°C, the protective group mixture in the three-necked flask A was added dropwise, and the temperature was controlled at -50°C for 2 hours to obtain cefprozil. The reaction to produce cefprozil Add 100mL crude cefprozil refined mother liquor and 11mL saturated FeCl 3 The solution, add hydrochloric acid to adjust the pH value to 0.8, raise the temperature to 8°C, stir for 30min, stand still, separate the liquids, cool the water phase to below -5°C, control the t...

Embodiment 3

[0047] Take 28.4g of 7-APRA, add 200mL of dichloromethane, 15.3g of hexamethyldisilazane, 9.8g of trimethylchlorosilane and 1g of imidazole to the three-necked flask A, and heat to reflux for 3h;

[0048] Take 91.2g of p-hydroxyphenylglycine Deng potassium salt, add 200mL of dichloromethane and 150mL of DMF to a three-necked flask B, drop the temperature to -50℃, add ethyl chloroformate, and control the temperature to -33℃-43℃ for 3h;

[0049] After the reaction, the active ester in the three-neck flask B was cooled to below -50°C, the protective group mixture in A was added dropwise, and the temperature was controlled at -50°C for 2 hours to prepare cefprozil. The cefprozil prepared reaction solution was added 120mL cef ℃ propylene crude refined mother liquor and 10mL saturated FeCl 3 The solution, add hydrochloric acid to adjust the pH value to 0.9, raise the temperature to 6, stir for 30min, stand still, separate, cool the water phase to below -5℃, add dimethylformamide and aceto...

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Abstract

The invention discloses a cefprozil mother liquor application technique, comprising the steps of (1) adding saturated FeCl3 solution into cefprozil mother liquor to adjust pH; (2) after cefprozil synthetic reaction is over, adding the cefprozil mother liquor treated in step (1) into the reaction liquid, raising the temperature, stirring at a controlled temperature, allowing standing, and dividingthe liquid; (3) cooling an aqueous layer divided from step (2) to below -5 DEG C, adding dimethylformamide at a controlled temperature, adding acetone washing liquid, stirring, filtering, and collecting filtrate; (4) cooling the filtrate, dropwise adding liquid ammonia to adjust pH, cooling, stirring, filtering, collecting filter cake, washing with dimethylformamide, washing with acetone, and drying in the vacuum to obtain crude cefprozil; and (5) refining the crude cefprozil. The cefprozil mother liquor application technique is simple and convenient to perform, usage of dimethylformamide andacetone is greatly reduced, and the cefprozil mother liquor application technique has significant economic and environmental benefits.

Description

Technical field [0001] The invention relates to the technical field of medicine, in particular to a cefprozil mother liquor application process. Background technique [0002] Cefprozil (Cefprozil) Chemical name: (6R,7R)-7 [(R)-2-amino-2-(p-hydroxy-phenyl)acetamido]-8-oxo-3-propene-5-thia -1-Azabicyclo-(4,2,0)oct-2-ene-2 ​​carboxylic acid-purified hydrate, developed by Bristol-Myer Squibb and listed in the United States in 1992 The second generation of new broad-spectrum oral cephalosporins are commonly used in adult upper and lower respiratory tract infections, urinary tract infections and intestinal infections, children's otitis media, tonsillitis, pneumonia and other upper and lower respiratory tract infections, urinary system infections and intestinal infections. They are currently used in industrial production. In the process, a certain amount of cefprozil often remains in the cefprozil mother liquor and washing liquid after synthesis and extraction. If it is not recycled, i...

Claims

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Application Information

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IPC IPC(8): C07D501/22C07D501/06
CPCC07D501/06C07D501/22
Inventor 杨明王俊臣樊振巩玉荣张垒钱丹吉令杨秋燕陈风高明靳朋飞殷恒亮赵臻
Owner TOPFOND PHARMA CO LTD
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