1/4 water ceftezole sodium compound

A technology of ceftezole sodium and its compound, which is applied in the field of 1/4 water ceftezole sodium compound and its preparation method, and can solve the problems of unsuitable storage, high environmental humidity requirements, poor stability, etc.

Inactive Publication Date: 2019-01-08
刘兆娟
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the methods for preparing ceftezole sodium all have high hygroscopicity, poor fluidity, and poor stability. In

Method used

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  • 1/4 water ceftezole sodium compound
  • 1/4 water ceftezole sodium compound

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Embodiment 1: Preparation of 1 / 4 water ceftezole sodium compound

[0025] At room temperature, dissolve 75.02g of sodium citrate in a mixture of 400ml of acetonitrile and 200ml of water, then add 100.05g of ceftezole and stir to dissolve, adjust the pH value to 4.0 with citric acid, add 6.12g of activated carbon, stir and adsorb for 30 minutes , decarbonized by suction filtration; washed the filter cake with 50ml of acetonitrile; lowered the temperature of the filtrate to 10°C, slowly added dichloromethane dropwise for 2h under stirring, filtered under reduced pressure, washed the filter cake with 50ml of dichloromethane, and dried under reduced pressure at 45°C After 4 hours, 83.26 g of ceftezole sodium compound in 1 / 4 water was obtained.

[0026] The powder X-ray diffraction pattern has characteristic diffraction peaks at the diffraction angles 2θ of 9.05°, 18.18°, 18.92°, 21.53°, 22.17°, 23.55°, and 24.71°, and the relative diffraction intensities of the diffraction ...

Embodiment 2

[0029] Embodiment 2: Preparation of 1 / 4 water ceftezole sodium compound

[0030] At room temperature, dissolve 75.05g of sodium citrate in 400ml of acetonitrile and 100ml of water mixture, then add 100.02g of ceftezole and stir to dissolve, adjust the pH value to 5.0 with citric acid, add 5.03g of activated carbon and stir for 30 minutes to adsorb , decarbonized by suction filtration; washed the filter cake with 50ml of acetonitrile; lowered the temperature of the filtrate to 0°C, slowly added dichloromethane dropwise under stirring for 2h, filtered under reduced pressure, washed the filter cake with 50ml of dichloromethane, and dried under reduced pressure at 40°C After 3.5 hours, 81.55 g of ceftezole sodium compound in 1 / 4 water was obtained.

[0031]The powder X-ray diffraction pattern has characteristic diffraction peaks at the diffraction angles 2θ of 9.08°, 18.16°, 18.93°, 21.57°, 22.20°, 23.57°, and 24.75°, and the relative diffraction intensities of the diffraction ang...

Embodiment 3

[0034] Embodiment 3: Preparation of 1 / 4 water ceftezole sodium compound

[0035] At room temperature, dissolve 75.01g of sodium citrate in 450ml of acetonitrile and 150ml of water mixture, then add 100.06g of ceftezole and stir to dissolve, adjust the pH value to 4.5 with citric acid, add 6.07g of activated carbon and stir for 30 minutes to adsorb , decarbonized by suction filtration; washed the filter cake with 50ml of acetonitrile; lowered the temperature of the filtrate to 5°C, slowly added dichloromethane dropwise with stirring for 2h, filtered under reduced pressure, washed the filter cake with 50ml of dichloromethane, and dried under reduced pressure at 50°C After 3 hours, 85.06 g of ceftezole sodium compound in 1 / 4 water was obtained.

[0036] The powder X-ray diffraction pattern has characteristic diffraction peaks at the diffraction angles 2θ of 9.03°, 18.19°, 18.90°, 21.50°, 22.15°, 23.52°, and 24.70°, and the relative diffraction intensities of the diffraction angle...

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PUM

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Abstract

The invention discloses a 1/4 water ceftezole sodium compound and a preparation method of the 1/4 water ceftezole sodium compound, and each molar of ceftezole sodium contains 1/4 molar of water. The inventor dissolves ceftezole acid into a mixed solution of acetonitrile and water, the pH and the temperature of the solution are controlled, dichloromethane is added to crystalize, and the 1/4 water ceftezole sodium compound is prepared. The 1/4 water ceftezole sodium compound is good in stability, high in purity, low in hygroscopicity, and good in flowability.

Description

technical field [0001] The invention belongs to the technical field of chemical engineering medicine crystallization, and relates to a 1 / 4 water ceftezole sodium compound and a preparation method thereof. Background technique [0002] Ceftezole sodium is the first generation of cephalosporin antibiotics. The mechanism of action is to inhibit the synthesis of bacterial cell walls to exert antibacterial activity. Bacteria such as Escherichia coli, Salmonella, Shigella, Proteus, etc. have antibacterial activity, and are mainly used for bronchitis, pneumonia and other respiratory tract infections, urinary tract infections, biliary tract infections, infections and sepsis caused by surgery, etc. [0003] The existing preparation methods of ceftezole sodium are as follows: CN 102010430 A, a synthesis process of ceftezole sodium; CN101735250 A, a new route of ceftezole sodium compound; CN 102010431 A, a ceftezole sodium compound and its new preparation CN 102219795 A preparation me...

Claims

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Application Information

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IPC IPC(8): C07D501/36C07D501/04C07D501/12A61K31/546A61P31/04
CPCC07B2200/13C07D501/04C07D501/12C07D501/36
Inventor 刘兆娟
Owner 刘兆娟
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