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1/2 water ceftezole sodium compound

A technology of ceftazole sodium and compound, applied in the field of 1/2 water ceftazole sodium compound and preparation method thereof, can solve the problems of poor fluidity and high hygroscopicity of ceftazole sodium

Inactive Publication Date: 2019-01-08
HAINAN LINGKANG PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the ceftezole sodium prepared by the prior art still has poor fluidity and high hygroscopicity.

Method used

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  • 1/2 water ceftezole sodium compound

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Embodiment 1: the preparation of 1 / 2 water ceftezole sodium compound

[0029] Measure 600ml of isopropanol and 100ml of water into the reaction kettle, under stirring, add 60.03g of ceftezole, control the temperature at 25°C, then slowly add sodium acetate, when the pH value is 7, stop adding, add 0.61g of activated carbon , decolorize by adsorption for 30min, decarbonize by filtration, wash the filter cake with 50ml of isopropanol×2; add the filtrate to the reaction kettle, add 500ml of ether under slow stirring, lower the temperature to 5°C, add dropwise 100ml of 2:1 ethanol and butyl The ketone mixture was stirred and crystallized for 2 hours, filtered with suction, the filter cake was washed with 50ml of ethanol × 2, and dried under reduced pressure at 40°C for 1.5 hours to obtain 46.9g of 1 / 2 water ceftezole sodium compound.

[0030] The powder X-ray diffraction pattern has characteristic diffraction peaks at the diffraction angles 2θ of 9.02°, 18.15°, 18.89°, 21.5...

Embodiment 2

[0033] Embodiment 2: Preparation of 1 / 2 water ceftezole sodium compound

[0034] Measure 700ml of isopropanol and 100ml of water into the reaction kettle, under stirring, add 60.11g of ceftezole, control the temperature at 15°C, then slowly add sodium acetate, when the pH value is 8, stop adding, add 0.63g of activated carbon , adsorption and decolorization for 30min, decarbonization by filtration, and washing the filter cake with 50ml of isopropanol×2; put the filtrate into the reaction kettle, add 500ml of diethyl ether under slow stirring, lower the temperature to 10°C, and dropwise add 100ml of 3:1 ethanol and butyl The ketone mixture was stirred and crystallized for 2.5 hours, filtered with suction, the filter cake was washed with 50ml of ethanol × 2, and dried under reduced pressure at 45°C for 2 hours to obtain 45.5g of 1 / 2 water ceftezole sodium compound.

[0035] The powder X-ray diffraction pattern has characteristic diffraction peaks at the diffraction angles 2θ of ...

Embodiment 3

[0038] Embodiment 3: Preparation of 1 / 2 water ceftezole sodium compound

[0039] Measure 800ml of isopropanol and 100ml of water into the reaction kettle, under stirring, add 60.07g of ceftezole, control the temperature at 35°C, then slowly add sodium acetate, stop adding when the pH value is 7.5, and add 0.64g of activated carbon , adsorption and decolorization for 30 minutes, decarbonization by filtration, washing the filter cake with 50ml of isopropanol×2; adding the filtrate to the reaction kettle, adding 500ml of ether under slow stirring, lowering the temperature to 15°C, and adding dropwise 100ml of 2.5:1 ethanol and butyl The ketone mixture was stirred and crystallized for 3 hours, filtered with suction, the filter cake was washed with 50ml of ethanol × 2, and dried under reduced pressure at 50°C for 1 hour to obtain 47.3g of 1 / 2 water ceftezole sodium compound.

[0040] The powder X-ray diffraction pattern has characteristic diffraction peaks at the diffraction angles...

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Abstract

The invention discloses a 1 / 2 water ceftezole sodium compound and a preparation method of the 1 / 2 water ceftezole sodium compound, and each molar of ceftezole sodium contains 1 / 2 molar of water. The low-hygroscopicity high-purity 1 / 2 water ceftezole sodium compound having good thermodynamic stability is finally prepared by adsorbing by using an activated carbon, controlling the pH and the crystallization temperature and using a specific solvent. The defects of high hygroscopicity, poor purity and poor thermodynamic stability of the raw material produced in the prior art are overcome, and the 1 / 2 water ceftezole sodium compound has a broader application prospect.

Description

technical field [0001] The invention belongs to the technical field of chemical engineering medicine crystallization, and relates to a 1 / 2 water ceftezole sodium compound and a preparation method thereof. Background technique [0002] Ceftezole sodium is the first generation of broad-spectrum cephalosporin antibiotics. It was first developed by Fujisawa Company in Japan. It exerts antibacterial activity by inhibiting the synthesis of bacterial cell walls. , Streptococcus pneumoniae, Streptococcus pyogenes, etc. have antibacterial activity, clinically mainly used for respiratory tract infection, urinary system infection, biliary tract infection, traumatic infection, superficial suppurative infection, gynecological infection, ENT infection, etc. [0003] There are many methods for preparing ceftezole sodium now. For example, CN 102219795A adopts a "one-pot" process. First, demethiadiazole reacts with 7-ACA to obtain TZT, then tetrazoleacetic acid and pivaloyl chloride generate...

Claims

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Application Information

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IPC IPC(8): C07D501/36C07D501/04A61K31/546A61P31/04
CPCC07D501/36
Inventor 黄奋
Owner HAINAN LINGKANG PHARMA CO LTD
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