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One-pot method for preparing ceftazidime

A technology for ceftazidime and aminocephalosporanic acid, which is applied in the field of medicine, can solve the problems such as prolonging the time required for the synthesis process, unsatisfactory product yield, increasing production cost and the like, and achieves avoiding the crystal growing process, reducing the workload and simplifying the treatment process. Effect

Inactive Publication Date: 2016-05-18
上海博速医药科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although this method simplifies the technological process, the product yield is not ideal, the yield is below 80%, and the highest purity can only reach 99.3%, which is far from enough for medicines
In addition, the protection and deprotection steps of functional groups are still involved, which will inevitably prolong the time required for the entire synthesis process and increase the production cost.

Method used

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  • One-pot method for preparing ceftazidime

Examples

Experimental program
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Effect test

Embodiment 1

[0022] The method for preparing ceftazime by one-pot method of the present invention comprises the steps of: weighing 2.72g of 7-aminocephalosporanic acid (7-ACA, compound I, MW272, 0.01mol), 3.28g of ceftazidime side chain acid chloride hydrochloride (compound II, MW328 , 0.01mol) and 9.48g pyridine (MW79, 0.12mol), placed in an ultrasonic reactor, -18 ° C, 750W ultrasonic vibration for 2 hours and 2 hours, adjust the pH to 4.1, add 1.632g acetone to the reaction solution, and white The solid was washed with cold water at 0°C, and vacuum-dried at 40°C for 4 hours to obtain 6.22g ceftazidime (MW636), with a yield of 97.8%, a purity of more than 99.9%, a single impurity of less than 0.01%, and acetone residue of less than 0.01%.

Embodiment 2

[0024] The method for preparing ceftazime by one-pot method of the present invention comprises the steps of: weighing 2.72g of 7-aminocephalosporanic acid (7-ACA, compound I, MW272, 0.01mol), 3.936g of ceftazidime side chain acid chloride hydrochloride (compound II, MW328 , 0.012mol) and 11.06g pyridine (MW79, 0.14mol), placed in an ultrasonic reactor, -15 ° C, 1000W ultrasonic vibration for 3 hours, adjust the pH to 4.2, add 2.176g acetone to the reaction solution, and precipitate a white solid, Wash with cold water at 5°C, and dry in vacuum at 50°C for 6 hours to obtain 6.24g of ceftazidime (MW636), with a yield of 98.1%, a purity of more than 99.9%, a single impurity of less than 0.01%, and acetone residue of less than 0.01%.

Embodiment 3

[0026] The method for preparing ceftazime by one-pot method of the present invention comprises the steps of: weighing 2.72g of 7-aminocephalosporanic acid (7-ACA, compound I, MW272, 0.01mol), 3.608g of ceftazidime side chain acid chloride hydrochloride (compound II, MW328 , 0.011mol) and 10.27g pyridine (MW79, 0.13mol), placed in an ultrasonic reactor, -16 ° C, 800W ultrasonic vibration for 2 hours, adjust the pH to 4.2, add 1.904g acetone to the reaction solution, and precipitate a white solid, Wash with cold water at 5°C, and dry in vacuum at 50°C for 5 hours to obtain 6.28g of ceftazidime (MW636), with a yield of 98.7%, a purity of more than 99.9%, a single impurity of less than 0.01%, and acetone residue of less than 0.01%.

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Abstract

The invention discloses a one-pot method for preparing ceftazidime. The one-pot method includes the steps that 7-aminocephalosporanic acid, ceftazidime side chain acyl chloride hydrochloride and pyridine are weighed, placed in an ultrasonic wave reactor and ultrasonically oscillated for 2-3 h at the temperature of minus 18 DEG C-minus 15 DEG C and the power of 750-1000 W, the pH value is adjusted to 4.1-4.2, acetone is added into a reaction solution, and a white solid is separated, washed with cold water at the temperature of 0 DEG C-5 DEG C and dried to obtain ceftazidime. In the method, pyridine serves as an acid-binding agent and a catalyst for an acyl chloride and amidogen reaction, a reactant and reaction solvent, other reagents are not added any more, and the workload of impurity research in the later period of new drug research is greatly reduced. By means of environment-friendly ultrasonic oscillation, after the reaction is completed, the processing process is simple, the long crystal growing process is avoided, and meanwhile the possible influence on product quality by acetone residual amount due to acetone washing after cold water washing is avoided. The yield and the purity are high, and the method is suitable for industrial production.

Description

technical field [0001] The invention relates to a preparation method, in particular to a one-pot method for preparing ceftazime. It belongs to the field of medical technology. Background technique [0002] Ceftazidime is a semi-synthetic third-generation cephalosporin. The product is free acid (pentahydrate), and a certain amount of anhydrous sodium carbonate is added to make injection for use. It is suitable for sepsis caused by sensitive Gram-negative bacilli, lower respiratory system infection, abdominal cavity and biliary system infection, complicated urinary tract infection and severe skin and soft tissue infection. [0003] Ceftazidime was discovered in 1978. In 1983, the British Glaxo Company first developed it and listed it on the market. In 1992, ceftazidime was listed for the first time in my country, and in 1993 it was officially included in the list of essential medicines in my country. After more than 10 years of clinical application verification, ceftazidi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D501/46C07D501/06C07D501/04
CPCC07D501/04C07D501/06C07D501/46
Inventor 方瑛
Owner 上海博速医药科技有限公司
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