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Novel crystal form of cefamandole nafate compound and crystal preparation method thereof

A technology for cefamandole sodium and compound, which is applied in the field of pharmaceutical separation, can solve the problems of unsolved solubility, unstable crystal water, many insoluble particles, etc., achieves easy commercial industrialization scale implementation, is conducive to long-term storage, and has high fluidity. Good results

Active Publication Date: 2015-04-22
TIANJIN UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Chinese patent CN201010257886.X and Chinese patent CN201010199235.X are both prepared hydrates, but substances containing crystal water often have the defect of unstable crystal water in the preparation process, such as the long-term test and accelerated test of Chinese patent CN201010257886.X The stability of sodium benzoate is significantly reduced, and sodium benzoate is added to the preparation claimed by Chinese patent CN201010199235.X, and sodium benzoate has potential safety hazards as a preservative, which has been banned in some countries
The compound of cefamandole sodium disclosed in Chinese patent 201210284600.6 does not solve the problem of solubility, and there are many insoluble particles, and a large amount of sodium carbonate is added to the preparation, or lidocaine, reduced glutathione and glutamine are added Lidocaine and reduced glutathione are both active drugs, and there are uncertain safety risks when used together

Method used

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  • Novel crystal form of cefamandole nafate compound and crystal preparation method thereof
  • Novel crystal form of cefamandole nafate compound and crystal preparation method thereof
  • Novel crystal form of cefamandole nafate compound and crystal preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] 0.40g of dry cefmendol sodium solid was added to 10mL of 1,4-dioxane to form a suspension, the suspension was stirred at a stirring rate of 600r / min, and the suspension was heated to 40°C, constant Temperature, stir the suspension for 5h, then cool the suspension to 5℃ at a rate of 0.2℃ / min, stir the suspension for 5h at a constant temperature, vacuum filter the crystal slurry, dry the product at 20℃, normal pressure for 6h to constant The new crystal form of cefmendol sodium was obtained. The X-ray powder diffraction pattern of the product is at diffraction angle 2θ=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 , There is a characteristic peak at 34.16°C, and DSC has an endothermic peak at 164°C. The new crystal form product obtained by this method has a melting point about 69°C higher than that of the common crystal form, and has higher thermal stability. It has no degradation and changes...

Embodiment 2

[0025] Add 0.43 g of dry cefmendol sodium solid to 4 mL of methanol to form a suspension, stir the suspension at a stirring rate of 800 r / min, and heat the suspension to 45° C., at a constant temperature, and stir the suspension for 8 hours. Then the temperature of the suspension was lowered to 10℃ at a rate of 1℃ / min, the suspension was stirred for 9h at a constant temperature, the crystalline slurry was vacuum filtered, and the product was dried at 40℃ and normal pressure for 10h to constant weight to obtain cefmandol Sodium crystal products. The X-ray powder diffraction pattern of the product is at diffraction angle 2θ=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 , There is a characteristic peak at 34.16°C, and the DSC analysis chart has an endothermic peak at 166°C. The new crystal form product obtained by this method has a melting point about 71°C higher than that of the common stable crysta...

Embodiment 3

[0027] Add 0.50 g of dry cefmendol sodium solid to 10 mL of ethyl acetate to form a suspension, stir the suspension at a stirring rate of 1000 r / min, and heat the suspension to 48° C., at a constant temperature, and stir the suspension After 9 hours, the temperature of the suspension was lowered to 15°C at a rate of 1°C / min, the suspension was stirred at a constant temperature for 8 hours, and the crystal slurry was vacuum filtered. The product was dried at 60°C and normal pressure for 10 hours to a constant weight to obtain cefmeng Polyester sodium crystal product. The X-ray powder diffraction pattern of the product is at diffraction angle 2θ = 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 , There is a characteristic peak at 34.22°C, and the DSC analysis chart has an endothermic peak at 164°C. The new crystal form product obtained by this method has a melting point of about 69°C higher than that ...

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Abstract

The invention relates to a novel crystal form of a cefamandole nafate compound and a crystal preparation method thereof. Characteristic peaks at diffraction angles 2theta and DSC are defined by using an X-ray powder diffraction map. The preparation method of crystals with novel crystal form of the cefamandole nafate compound comprises the following steps: adding a cefamandole nafate solid into an organic solvent to prepare a 0.04-0.3g / ml suspension; stirring and suspending for a while at 40-50 DEG C; then, cooling to 5-15 DEG C at a certain cooling rate for a while; carrying out suction filtration on the suspension to obtain a filter cake which is a cefamandole nafate wet product; and drying the cefamandole nafate wet crystal product to constant weight so as to obtain a final novel crystal form product of the cefamandole nafate compound. The novel crystal form product has good thermal stability and is hardly deteriorated when being stored. Meanwhile, the novel crystal form is in a shape of a thick rod and has good mobility and high bulk density, so that the packaging and transporting convenience of the product is remarkably improved.

Description

Technical field [0001] The invention belongs to the technical field of medicine separation, and particularly relates to a new crystal form of a cefmendol sodium compound and a preparation method thereof. Background technique [0002] The chemical name of Cefamandole nafate is 7-D-(2-formyloxyphenylacetamide)-3-[(1-methyl-1H-tetrazol-5-yl)thiomethyl] -8-oxo-5-thia-1-azabicyclo[4.2.0]oct-2-ene-2-carboxylate sodium salt, the molecular formula is C 19 H 18 N 6 NaO 6 S 2 , The molecular weight is 512.50. The structural formula is as formula (I). [0003] [0004] Cefmendol Sodium was developed by Lilly Corporation of the United States in 1972, and was first marketed in 1978. The injection product is called MANDOL. Cefmendolin sodium is a second-generation semi-synthetic cephalosporin with strong bactericidal effect. It has some advantages of the first and third-generation cephalosporins. It is stable to β-lactamase and has low nephrotoxicity. , High blood concentration, good tissue p...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D501/36C07D501/12A61P31/04
CPCC07D501/12C07D501/36A61P31/04C07B2200/13
Inventor 郝红勋陶灵刚何芳侯宝红吕军尹秋响王永莉龚俊波谢闯鲍颖
Owner TIANJIN UNIV
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