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Synthesis method of ceftazidime impurity H

A ceftazidime and synthetic method technology, applied in the field of medicinal chemistry, can solve the problems such as few reports on the synthetic process of impurity H, and achieve the effects of good separation, easy preparation and high product purity

Inactive Publication Date: 2019-01-18
SHANGHAI NEW ASIA PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Therefore, the ceftazidime impurity H sample needs to be analyzed and detected as a reference substance in the quality detection of ceftazidime, but the synthesis process of impurity H is seldom reported

Method used

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  • Synthesis method of ceftazidime impurity H

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] 30g of ceftazidime hydrochloride was dropped into 100ml of methanol solution, and the reaction temperature was controlled to 30°C. After the solution was completely clarified, 10ml of concentrated hydrochloric acid was added and reacted for 48h. The reaction solution was filtered, and the filter cake was washed with 5 ml of methanol and sucked dry. The resulting solid was recrystallized twice from 95% methanol solution to obtain 5.3 g of white crystals with a purity of 90%.

Embodiment 2

[0034] 20g of ceftazidime hydrochloride was dropped into 100ml of methanol solution, and the reaction temperature was controlled to 40°C. After the solution was completely clarified, 10ml of concentrated hydrochloric acid was added and reacted for 72h.

[0035] The reaction solution was cooled to 25°C, filtered, and the filter cake was washed with 5 ml of methanol and sucked dry. The resulting solid was recrystallized once from 95% methanol solution to obtain 6 g of white crystals with a purity of 95%.

[0036] The structure of the above-mentioned ceftazidime impurity H is confirmed as follows:

[0037] EMS:[M+H] + is m / z561.12;

[0038] IR (cm -1 ):3415,3291,1776,1734,1663,1627,1536,1385,1151;

[0039] 1 H-NMR (D 2 O,400MHz):1.34(s,6H),3.00(d,J=18Hz,1H),3.42(d,J=18Hz,1H),3.54(s,3H),5.06(d,J=5Hz,1H ),5.34(d,J=14Hz,1H),5.35(d,J=14Hz,1H),5.66(d,J=5Hz,1H),6.79(s,1H),7.86(t,J=7Hz, 2H), 8.34(t, J=7Hz, 1H), 8.74(d, J=5Hz, 2H);

[0040] 13 C-NMR (D 2 (0,400MHz): δ176.3, 1...

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Abstract

The invention provides a synthesis method of a ceftazidime impurity H. The method is characterized by carrying out esterification reaction of ceftazidime hydrochloride in the presence of acid at the temperature below 20-40 DEG C to obtain the ceftazidime impurity H. The ceftazidime impurity H prepared by the method is more convenient to prepare and high in purity; the guarantee is provided for detection and research of the impurity quality of ceftazidime products.

Description

technical field [0001] The invention relates to the field of medicinal chemistry, in particular to a method for synthesizing ceftazidime impurity H. Background technique [0002] Ceftazidime is a third-generation cephalosporin antibiotic. It is used for sepsis, lower respiratory tract infection, abdominal cavity and biliary tract infection, complicated urinary tract infection and severe skin and soft tissue infection caused by sensitive Gram-negative bacilli. It is especially suitable for infection of immunocompromised persons caused by multiple drug-resistant Gram-negative bacilli, nosocomial infections, and central nervous system infections caused by Gram-negative bacilli or Pseudomonas aeruginosa. After single intravenous infusion and intravenous injection of 1 g ceftazidime in adults, the peak plasma concentration (Cmax) can reach 70-72 mg / L and 120-146 mg / L respectively, and the blood drug elimination half-life (t1 / 2β) is about 1.5-2.3 hours . [0003] Ceftazidime ha...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D501/46C07D501/04
CPCC07D501/04C07D501/46
Inventor 胡国栋崔万胜商鼎
Owner SHANGHAI NEW ASIA PHARMA
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