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Novel crystalline form of cefamandole nafate compound, preparation and preparing method thereof

a cefamandole nafate and compound technology, applied in the field of medicine separation technology, can solve the problems of uncertain security risks of lidocaine and reduced glutathione active drugs, and achieve the effects of improving thermal stability, improving form, and high melting poin

Inactive Publication Date: 2017-12-07
YINING AIERXING INTELLETUAL PROPERTY SERVICE CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Benefits of technology

[0017]Said method has the following advantageous effects: simple procedure, easy operation, and low energy consumption. The prepared product has a melting range of 160˜170° C. with good thermal stability, and is conducive to the long-term preservation. The product has a purity of 99% or above with a yield of 90% or higher, and the purity, the color and the appearance do not make any change after 100 days storing at normal temperature under dry condition. The product is easy to crush and processed into dosage forms of a pharmaceutical composition, as well as low cost, and easier to implement on commercial and industrial scale.
[0018]The novel crystalline form of Cefamandole Nafate obtained from said method has higher melting point and better thermal stability than those of reported forms, without degradation after placing for a long time. The product has better form, higher bulk density, better mobility, more uniform particle size distribution, and more conducive to post-treatment, which make great advantages in pharmaceutical formulations. Meanwhile, the product has a high purity and a high process yield.
[0019]It is shown on toxic reactions that the novel crystalline form of Cefamandole Nafate compound provided in the present invention has decreased toxicity than that of existing Cefamandole Nafate.

Problems solved by technology

Meanwhile, a lot of sodium carbonate, lidocaine, reduced glutathione or sodium glutamate are added in the formulation, and lidocaine and reduced glutathione are active drugs with uncertain security risks when they are used with Cefamandole Nafate.

Method used

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  • Novel crystalline form of cefamandole nafate compound, preparation and preparing method thereof
  • Novel crystalline form of cefamandole nafate compound, preparation and preparing method thereof
  • Novel crystalline form of cefamandole nafate compound, preparation and preparing method thereof

Examples

Experimental program
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Effect test

example 1

[0024]0.40 g of Cefamandole Nafate as dried solid was added to 10 mL of 1,4-dioxane to form a suspension, stirring the suspension at 600 r / min and heating to 40° C., continuing to stir for 5 h under constant temperature, and then cooling the suspension down to 5° C. at a cooling rate of 0.2° C. / min and stirring for 5 h under constant temperature, vacuum filtrating the crystal slurry, and the residue was dried at 20° C. and under normal pressure for 6 h to constant weight, to obtain a product of novel crystalline form of Cefamandole Nafate. The XRD pattern of the product was shown in FIG. 1, having characteristic peaks expressed in degrees 2θ at 4.01, 4.66, 6.18, 7.47, 9.95, 10.70, 14.56, 15.82, 16.26, 17.40, 18.05, 19.26, 20.15, 21.45, 22.25, 22.78, 24.00, 24.94, 30.17, and 34.16. The DSC thermogram was shown in FIG. 2, having an endothermic peak at 164° C. The product of the novel crystalline form provided by this method had a melting point, which is about 69° C. higher than that o...

example 2

[0025]0.43 g of Cefamandole Nafate as dried solid was added to 4 mL of methanol to form a suspension, stirring the suspension at 800 r / min and heating to 45° C., continuing to stir for 8 h under constant temperature, and then cooling the suspension down to 10° C. at a cooling rate of 1° C. / min and stirring for 9 h under constant temperature, vacuum filtrating the crystal slurry, and the residue was dried at 40° C. and under normal pressure for 10 h to constant weight, to obtain a product of novel crystalline form of Cefamandole Nafate. The XRD pattern of the product had characteristic peaks expressed in degrees 2θ at 4.04, 4.70, 6.22, 7.48, 9.90, 10.80, 14.66, 15.72, 16.22, 17.38, 18.02, 19.20, 20.08, 21.38, 22.12, 22.82, 23.88, 24.92, 30.32, 34.16. The DSC thermogram had an endothermic peak at 166° C. The product of the novel crystalline form provided by this method had a melting point, which is about 71° C. higher than that of a common crystal form, with higher thermal stability, ...

example 3

[0026]0.50 g of Cefamandole Nafate as dried solid was added to 10 mL of ethyl acetate to form a suspension, stirring the suspension at 1000 r / min and heating to 48° C., continuing to stir for 9 h under constant temperature, and then cooling the suspension down to 15° C. at a cooling rate of 1° C. / min and stirring for 8 h under constant temperature, vacuum filtrating the crystal slurry, and the residue was dried at 60° C. and under normal pressure for 10 h to constant weight, to obtain a product of novel crystalline form of Cefamandole Nafate. The XRD pattern of the product had characteristic peaks expressed in degrees 2θ at 4.10, 4.76, 6.28, 7.54, 9.98, 10.61, 14.46, 15.62, 16.30, 17.46, 18.08, 19.28, 20.16, 21.48, 22.26, 22.84, 24.00, 24.98, 30.26, 34.22. The DSC thermogram had an endothermic peak at 164° C. The product of the novel crystalline form provided by this method had a melting point, which is about 69° C. higher than that of a common crystal form, with higher thermal stab...

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Abstract

A novel crystalline form is defined by diffraction angle 2θ° of X-ray powder diffraction pattern and characteristic peak of differential scanning calorimetry (DSC). The novel crystalline form of Cefamandole Nafate is prepared as follows: adding Cefamandole Nafate in solid state to an organic solvent to form a suspension with a concentration of 0.04˜0.3 g / ml, stirring the suspension at 40˜50° C. for a period of time, and then cooling to 5˜15° C. at certain cooling rate, continuing to stir for a period of time, then suction filtrating the obtained suspension, the resulting filer cake is Cefamandole Nafate as wet product, which is dried to constant weight to provide the novel crystalline form of Cefamandole Nafate as final product.

Description

[0001]This application is the continuation-in-part application claims priority to U.S. patent application Ser. No. 15 / 305,661 filed 21 Oct. 2016 that is the U.S. national phase of International Application No. PCT / CN2015 / 095229 filed on 20 Nov. 2015 which designated the U.S. and claims priority to Chinese Application Nos. CN201410784492.8 filed on 16 Dec. 2014, the entire contents of each of which are hereby incorporated by reference.FIELD OF THE INVENTION[0002]The invention belongs to the field of medicine separation technology, and in particular, relates to a novel crystalline form of Cefamandole Nafate compound and its preparing method.PRIOR ART[0003]Cefamandole Nafate has a chemical name of (6R,7R)-7-R-(2-formyloxy-2-phenylacetamide)-3-[[(1-methyl-1H-tetrazol-5-yl)thio]methyl]-8-oxo-5-thia-1-azabicyclo[4.2.0]oct-2-ene-2-carboxylate sodium salt with a formula of C19H17N6NaO6S2 and a molecular weight of 512.49, and the structure formula is shown in formula (I):[0004]Cefamandole Na...

Claims

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Application Information

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Patent Type & Authority Applications(United States)
IPC IPC(8): C07D501/36C07D501/12
CPCC07D501/36C07D501/12C07B2200/13C07D501/60
Inventor HAO, HONGXUNTAO, LINGGANGHE, FANGHOU, BAOHONGWANG, JINGKANGLV, JUNYIN, QIUXIANGWANG, YONGLIGONG, JUNBOXIE, CHUANGBAO, YING
Owner YINING AIERXING INTELLETUAL PROPERTY SERVICE CO LTD
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