Novel crystal form of cefuroxime sodium and preparation method of cefuroxime sodium crystal

A cefuroxime sodium and crystal form technology, applied in the field of chemical engineering crystallization, can solve problems such as short shelf life, poor thermal stability, and increased storage difficulty, achieve moderate pH, avoid yield loss, and reduce the cost of decolorization and filtration processes Effect

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

AI Technical Summary

Problems solved by technology

The existing crystalline products begin to decompose in the first stage at 195°C, with poor thermal stability, which increases the difficulty of storage and has a short shelf life

Method used

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  • Novel crystal form of cefuroxime sodium and preparation method of cefuroxime sodium crystal
  • Novel crystal form of cefuroxime sodium and preparation method of cefuroxime sodium crystal
  • Novel crystal form of cefuroxime sodium and preparation method of cefuroxime sodium crystal

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Add 5 g of cefuroxime acid into the crystallizer, and at the same time add 100 ml of methanol, and stir at 20°C. Then, a sodium lactate-methanol solution with a concentration of 0.3 g / ml was added into the crystallizer for reaction, and the pH value at the end of the reaction process was controlled at 6.0. Then dropwise add 500ml of ethanol eluent at a rate of 2ml / min. After the crystallization was completed, the crystal slurry was filtered, washed with ethanol, and the obtained crystal product was dried at 40° C. and 0.005 MPa for 5 hours. The one-way mass yield of the crystal product is 93.4%, and the purity is 99.54%. Its X-ray powder diffraction has characteristic peaks at diffraction angles 2θ=3.5, 10.6, 12.7, 18.6, 19.6, and 22.4 degrees. Characteristic peaks.

Embodiment 2

[0026] Add 2.5g of cefuroxime acid into the crystallizer, add 50ml of methanol and 50ml of ethanol at the same time, and stir at 23°C. Then, a sodium lactate-methanol solution with a concentration of 0.2 g / ml was added into the crystallizer for reaction, and the pH value at the end of the reaction process was controlled at 6.2. Then dropwise add 200ml of ethanol eluent at a rate of 0.5ml / min. After the crystallization was completed, the crystal slurry was filtered, washed with ethanol, and the obtained crystal product was dried at 40° C. and 0.01 MPa for 4 hours. The one-way mass yield of the crystal product is 94.7%, and the purity is 99.52%. Its X-ray powder diffraction has characteristic peaks at diffraction angles 2θ=3.4, 10.6, 12.6, 18.6, 19.4, and 22.4 degrees. Its DSC spectrum has Characteristic peaks.

Embodiment 3

[0028] Add 3g of cefuroxime acid into the crystallizer, add 50ml of methanol and 50ml of n-propanol at the same time, and stir at 23°C. Then, a sodium lactate-methanol solution with a concentration of 0.3 g / ml was added into the crystallizer for reaction, and the pH value at the end of the reaction process was controlled at 6.3. Then add 100ml ethanol and 150ml n-propanol eluent dropwise at a rate of 0.8ml / min. After the crystallization was completed, the crystal slurry was filtered, washed with ethanol, and the obtained crystal product was dried at 35° C. and 0.02 MPa for 3 hours. The one-way mass yield of the crystal product is 93.5%, and the purity is 99.59%. Its X-ray powder diffraction has characteristic peaks at diffraction angles 2θ=3.5, 10.8, 12.8, 18.6, 19.7, and 22.4 degrees, and its DSC spectrum has Characteristic peaks.

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Abstract

The invention provides a novel crystal form of cefuroxime sodium and a preparation method of cefuroxime sodium crystal. According to the novel crystal form crystal, the X-ray powder diffracting at the diffraction angles 2theta of 3.5+ / -0.2, 10.6+ / -0.2, 12.7+ / -0.2, 18.6+ / -0.2, 19.5+ / -0.2 and 22.4+ / -0.2 has characteristic peaks. The DSC graph has a characteristic peak at the angle of 235+ / -2 degrees. The method for preparing the novel cefuroxime sodium crystal comprises the following steps: adding 2.5-5g of cefuroxime acid with the purity of 99 percent into 100mL of a solvent for stirring at the temperature of 20-25 DEG C, drilling 0.2-0.4g / mL of sodium lactate-methanol solution for reacting until the pH value of the solution is 6.0-6.5; adding a solventing-out agent for performing solvent-out crystallization; and filtering, washing and drying the crystal mush, thereby obtaining the cefuroxime sodium crystallization product with the crystal form.

Description

technical field [0001] The invention belongs to the technical field of chemical engineering crystallization, and in particular relates to a new crystal form of cefuroxime sodium and a crystallization preparation method thereof. Background technique [0002] The chemical name of Cefuroxime sodium is (6R,7R)-7-[2-furyl(methoxyimino)acetamido]3-carbamoyloxymethyl-8-oxo-5- Thia-1-azabicyclo[4.2.0]oct-2-ene-2-carboxylic acid sodium salt, molecular formula C 16 h 15 N 4 NaO 8 S, the molecular weight is 446.37, and its chemical structure is shown below. [0003] [0004] Cefuroxime sodium is the best second-generation cephalosporin with the advantages of the first-generation and third-generation cephalosporins. Cefuroxime sodium has a significant effect on most Gram-positive and negative bacteria and some anaerobic bacteria, even against Methicillin-resistant enzyme-producing strains also have certain effects, and have the advantages of strong bactericidal activity, low tox...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D501/34C07D501/12
CPCC07D501/12C07D501/34
Inventor 王永莉王慧慧郝红勋侯宝红鲍颖谢闯王静康尹秋响龚俊波张美景
Owner TIANJIN UNIV
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