A kind of azlocillin sodium crystal and preparation method thereof

A technology of azlocillin sodium and crystal, applied to the crystal of azlocillin sodium and the field of preparation thereof, can solve the problem of improper solvent and elution agent dosage, high cost of industrialized production, easy agglomeration of azlocillin sodium, etc. problem, to achieve the effect of low production cost, short production cycle, and less toxic and side effects of drugs

Active Publication Date: 2019-02-22
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

CN 1778804A discloses a kind of crystalline azlocillin sodium and its preparation method, and this document provides its product XRD pattern to see attached figure 1 , its decomposition temperature is 224±1°C, but azlocillin sodium is easy to agglomerate during the drying process of the product in this method, and it can be used after being pulverized; and this method uses a large amount of mixed organic solvents, which makes the recovery of the solvent very difficult and increases cost of production
CN 103265561 A discloses azlocillin sodium compound and its preparation method, and this document provides its product XRD spectrum and sees attached figure 2 , the process is complicated and involves two cooling crystallizations; before the second cooling crystallization, the solution of azlocillin sodium is concentrated under reduced pressure to half of its original volume, which requires high energy consumption and high industrial production costs
CN 104130270 A discloses a new penicillin crystal preparation and its preparation method, the original text of this document figure 1 Given the XRD spectrum of its product, the yield of the product obtained by this method is only 76.3%, which may be due to the improper selection of solvent and eluent or too little amount of eluent, which needs further improvement

Method used

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  • A kind of azlocillin sodium crystal and preparation method thereof
  • A kind of azlocillin sodium crystal and preparation method thereof
  • A kind of azlocillin sodium crystal and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Add 3.75g of azlocillin sodium solid into 15mL of methanol, stir at 30°C until completely dissolved, then cool down to 10°C at a rate of 1.0°C / min, and add 30mL of n-propanol to the solution at a rate of 6.0ml / min , precipitated crystals, continued to stir for 6 hours, filtered with suction, and dried the obtained wet product at 25°C under normal pressure for 6 hours to obtain a new crystal form of azlocillin sodium. The X-ray powder diffraction pattern of the new crystal product is as follows: image 3 As shown, it has characteristic peaks at diffraction angles 2θ=4.92, 6.49, 7.20, 8.03, 9.18, 9.74, 10.56, 11.64, 12.91, 14.43, 15.39, 16.32, 16.57, 17.11, 17.83, 18.25, 18.90, 19.44 degrees; The TGA of the new crystalline product is as follows: Figure 4 As shown, the decomposition temperature is 217.0° C., and the solubility of the product is good; the crystal appearance is fusiform, the product purity is 99.6%, and the process yield is 95.4%.

Embodiment 2

[0035] Add 3.75g of azlocillin sodium solid into 15mL of water, stir at 30°C until completely dissolved, then cool down to 0°C at a rate of 2.0°C / min, add 90ml of ethanol to the solution at a rate of 9.0ml / min, and precipitate crystals , continue to stir for 6 hours, filter with suction, and dry the obtained wet product at 35°C under normal pressure for 3 hours to obtain a new crystal form of azlocillin sodium. , 10.49, 11.75, 12.99, 14.23, 15.28, 16.17, 16.57, 17.05, 17.86, 18.39, 19.08, and 19.51 degrees have characteristic peaks; the decomposition temperature of this new crystal form is 216.0°C, and the solubility of the product is good; the crystal appearance is Shuttle shape, product purity 99.3%, process yield 96.3%.

Embodiment 3

[0037]Add 3.00 g of azlocillin sodium solid into 15 mL of N.N-dimethylformamide, stir at 25 °C until completely dissolved, then cool down to 15 °C at a rate of 0.1 °C / min, and add to the Add 60mL of isobutanol to the solution to precipitate crystals, continue to stir for 2h, filter with suction, and dry the obtained wet product at 35°C and normal pressure for 3h to obtain a new crystal form of azlocillin sodium, which has a diffraction angle of 2θ= There are characteristic peaks at 5.08, 6.63, 7.21, 8.14, 9.38, 9.89, 10.76, 11.65, 12.97, 14.29, 15.26, 16.18, 16.62, 17.05, 17.79, 18.22, 18.95, and 19.47 degrees; the decomposition temperature of the new crystal is 218.0 °C, the solubility of the product is good; the crystal appearance is fusiform, the product purity is 99.4%, and the process yield is 96.2%.

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Abstract

The invention relates to a crystal form of azlocillin sodium and a preparation method thereof. The crystal form is characterized by TGA characteristic peaks in the diffraction angles 2 theta in the X-ray powder diffraction spectrum; the amoxicillin sodium solid is added into a good solvent at 20-30 DEG C, the axlocillin sodium is completely dissolved by stirring, and the concentration of the solution is 0.2-0.3 g / ml, the system temperature is reduced to 0-15 DEG C, a poor solvent is added, crystals are crystallised out, and stirring is continued for 2-10 hours, the crystal pulp is subjected to filtration, washing and drying to obtain the amoxicillin sodium crystal form product. The crystal form crystal is large in particle size and good in fluidity, and the decomposition temperature is 217 + / -1 DEG C, the solubility of the product is large, the solubility of the product is improved, and the absorption and utilization of the drug are facilitated.

Description

technical field [0001] The invention belongs to the technical field of purification and separation of antibiotic drugs, and in particular relates to a crystal of azlocillin sodium and a preparation method thereof. Background technique [0002] The chemical name of Azlocillin sodium is (2S, 5R, 6R)-3,3-dimethyl-6-[(R)-2-(2-oxo-1-imidazolidinecarboxamido )-2-phenylacetamido]-7-oxo-4-thia-1-azabicyclo[3.2.0]heptane-2-carboxylic acid sodium salt, the molecular formula is C 20 h 22 N 5 NaO 6 S, the molecular weight is 483.47. The structural formula is as formula (I). [0003] [0004] Azlocillin sodium was first developed by the German Bayer company, and it was listed for the first time in May 1977. The listed company: Badrich, and the product name: Cyclone. Since the 1980s, it has been used in Britain, the United States, Japan and other countries. It was included in the supplementary volume of the 20th edition of the United States Pharmacopoeia in 1983, and it was still...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D499/68C07D499/18
CPCC07B2200/13C07D499/18C07D499/68
Inventor 郝红勋周亚男侯宝红鲍颖王静康尹秋响张美景谢闯
Owner TIANJIN UNIV
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