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Novel ceftazidime compound
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A technology of ceftazidime and compounds, applied in the field of new ceftazime compounds and their preparation, new compounds and their preparations, can solve problems such as easy generation of impurities and unsatisfactory product stability
Inactive Publication Date: 2016-11-30
石药集团中诺药业(石家庄)有限公司
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CN201410126071.6 relates to a ceftazidime compound and its pharmaceutical composition, which discloses the diffraction data of the compound, but the stability of the product is still not ideal, and impurities are likely to be produced
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Embodiment 1
[0031] Embodiment 1 prepares new ceftazime compound of the present invention
[0032] Add 1000g of ceftazidime crude product into a 10L three-neck flask, add 5000mL of water and 800mL of dimethyl sulfoxide, stir and heat to reflux to dissolve, then add 800mL of chloroform to the solution, then slowly cool down to 10°C, stir and crystallize, filter , washed with methanol, and vacuum-dried at 45° C. to obtain 966 g of a new ceftazidime compound with a yield of 96.6%.
[0033] The X-raypowder diffraction pattern of the new ceftazidime compound at the reflection angle 2θ is (with an accuracy of ±0.1°): 4.93°, 5.87°, 7.02°, 7.83°, 8.34°, 9.72°, 12.21°, 13.01°, 13.97° , 14.52°, 15.58°, 16.43°, 17.39°, 17.83°, 18.57°, 19.01°, 19.42°, 19.97°, 20.52°, 20.91°, 21.28°, 21.88°, 22.91°, 23.56°, 24.50°, 24.92 °, 25.47°, 29.69° have characteristic absorption peaks, such as figure 1 shown.
[0034]Its DSC spectrum has a characteristic endothermic peak near 185.22°C (with an accuracy of ±1...
Embodiment 2
[0035] Embodiment 2 prepares new ceftazime compound of the present invention
[0036] Add 1000g of ceftazidime crude product into a 10L three-neck flask, add 4500mL of water and 1000mL of dimethyl sulfoxide, stir and heat to reflux to dissolve, then add 600mL of chloroform to the solution, then slowly cool down to 15°C, stir and crystallize, filter , washed with methanol, and vacuum-dried at 50° C. to obtain 945 g of a new ceftazidime compound with a yield of 94.5%.
Embodiment 3
[0037] Embodiment 3 prepares new ceftazidime compound of the present invention
[0038] Add 1000g of ceftazidime crude product into a 10L three-necked flask, add 6000mL of water and 500mL of dimethyl sulfoxide, stir and heat to reflux to dissolve, then add 1000mL of chloroform to the solution, then slowly cool down to 0°C, stir and crystallize, filter , washed with methanol, and vacuum-dried at 40° C. to obtain 923 g of a new ceftazidime compound with a yield of 92.3%.
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Abstract
The invention relates to a novel ceftazidime compound and a preparation method therefor, and belongs to the technical field of medicines. According to the novel ceftazidime compound, an X-raypowderdiffraction pattern obtained through carrying out measuring by using Cu-K alpha rays displays characteristic peaks when a 2[theta] angle is 4.93+ / -0.1 degrees, 7.02+ / -0.1 degrees, 7.83+ / -0.1 degrees, 8.34+ / -0.1 degrees, 13.01+ / -0.1 degrees and 21.88+ / -0.1 degrees. The novel ceftazidime compound prepared by the preparation method is good in fluidity, can better meet the requirements of pharmaceutics and is more suitable for preparing various pharmaceutical preparations. Sterile powder-injection preparations prepared from the novel ceftazidime compound disclosed by the invention are good in stability and are not added with cosolvents such as arginine, so that the safety and effectiveness of medication are improved, and the incidence rate of adverse reactions is lowered.
Description
technical field [0001] The invention relates to a novel compound and a preparation method thereof, in particular to a novel ceftazidime compound and a preparation method thereof, belonging to the technical field of medicine. Background technique [0002] Ceftazidime (Ceftazidime), whose chemical name is (6R,7R)-7-[[(2-amino-4-oxazolyl)-[(1-carboxy-1-methylethoxy)imino]acetyl ]Amino]-2-carboxy-8-oxo-5-thia-1-azabicyclo[4.2.0]oct-2-ene-3-methylpyridinium inner salt pentahydrate, molecular formula C 22 h 22 N 6 o 7 S 2 ·5H 2 O, the molecular weight is 636.65. The properties of ceftazime are white or off-white crystalline powder, odorless or slightly peculiar smell, slightly soluble in water or methanol, insoluble in acetone, slightly soluble in phosphate buffer (pH 6.0). Its chemical structural formula is: [0003] [0004] Ceftazidime is a semi-synthetic third-generation cephalosporin antibiotic with strong antibacterial activity and broad antibacterial spectrum, an...
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