Novel crystal form of cefuroxime acid and preparation method thereof

A technology of cefuroxime acid and crystal form, which is applied in the field of new crystal form of cefuroxime acid and its crystal preparation, can solve the problems of poor crystal form of cefuroxime acid, high labor intensity, difficulty in filtration and drying, etc., and achieves thermal stability Good, low labor intensity, complete crystal form effect
CN102746323AActive Publication Date: 2012-10-24TIANJIN UNIV
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Patent Information

Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
TIANJIN UNIV
Publication Date
2012-10-24

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Abstract

The invention relates to a novel crystal form of cefuroxime acid and a preparation method thereof. In X ray powder diffraction, the novel crystal form of cefuroxime acid has characteristic peaks at diffraction angles 2 theta of 8.06, 9.96, 10.44, 11.84, 12.82, 16.34, 19.02, 20.02, 21.86, 23.22, 25.46, 25.98, 33.12, 34.24 and 36.40 degrees. The preparation method comprises the following steps of adding cefuroxime raw materials into an acetonitrile mixed solvent to obtain a solution having a concentration of 0.1 to 0.2g / ml, stirring at a temperature of 25 to 35 DEG C for complete dissolution, continuously stirring for 30 to 60 minutes, carrying out filtration and decoloration, transferring filtrate to a crystallizer, adding a hydrochloric acid solution into the crystallizer to adjust a pH value of the mixed solution to 3-4, cooling to a temperature of 10 to 15 DEG C, adding cefuroxime acid seed crystals into the crystallizer, carrying out crystallization for 1 to 2 hours, adding water as a solventing-out agent into the crystallizer, sequentially cooling to a temperature of 0 to 5 DEG C, carrying out crystallization for 1 to 3 hours, filtering, washing filter cake by a washing solvent, and drying to obtain products. The novel crystal form of cefuroxime acid has HPLC content above 99.3%, avoids crystal accumulation, has large particle sizes, wherein a main particle size is more than 100 microns, and also has uniform particle size distribution and a single-cycle mole yield above 88% in crystallization.
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Description

Technical field

[0001] The invention belongs to the technical field of crystallization, and particularly relates to a new crystal form of cefuroxime acid and a crystal preparation method thereof. Background technique

[0002] The chemical name of Cefuroxime acid 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, molecular formula is C 16 H 16 N 4 O 8 S, molecular weight is 424.39, CAS number: 55268-75-2, and its chemical structure is shown below.

[0003]

[0004] Cefuroxime acid is an intermediate in the production of the second generation antibiotics cefuroxime sodium and cefuroxime axetil. Cefuroxime antibiotics are broad-spectrum antibiotics. They have obvious antibacterial activity against Gram-negative bacteria and Gram-positive bacteria. They can be used to treat respiratory infections, ear, nose, and throat infections, and urinary infections caused by sensitive bacteria. Tract infections, skin a...

Claims

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