Cadrofloxacin hydrochloride-I crystal and preparation method thereof

A technology of caltrafloxacin and hydrochloric acid calfloxacin, which is applied to the I-type crystal of caltrafloxacin hydrochloride and its preparation field, can solve the problems of unfavorable crystal structure, easy agglomeration, fine crystallization of products, etc. Good storage, good chemical stability and controllable product quality

Inactive Publication Date: 2010-07-14
SUNCADIA PHARM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Since the chemical structure of cadrofloxacin hydrochloride itself has both acidic and basic functional groups, the solubility of the product often changes with the pH of the solution, and the structure of the product itself is closely related to the pH of the solution during crystallization; Rapid elution or the use of adjusting acidity to precipitate products are not conducive to the regular crystal structure of the product, but also have other defects, such as fine crystallization of the product, difficult filtration, easy agglomeration, poor fluidity, etc. It also shows that fast washing and acid precipitation products can only be similar to amorphous solids, even if the products are separated out and stirred for a long time, only not very typical crystal absorption peaks can be seen on the X-diffraction spectrum, indicating that The product is mixed with some degree of amorphous product

Method used

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  • Cadrofloxacin hydrochloride-I crystal and preparation method thereof
  • Cadrofloxacin hydrochloride-I crystal and preparation method thereof
  • Cadrofloxacin hydrochloride-I crystal and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0024] Add 2.00 g of cadrofloxacin hydrochloride into water (50 ml), heat to reflux to dissolve, filter and slowly cool to crystallize, and collect the precipitated crystals by filtration. The obtained crystals were dried at 40° C. under reduced pressure for 3 hours to obtain 1.17 g of crystals with a yield of 58.5%. The resulting sample contained 0.53% moisture; the X-ray diffraction spectrum of the crystallized sample can be found in figure 1 , is a type I crystal. The crystallization at about 3.88 (22.75), 7.24 (12.20), 9.04 (9.77), 9.42 (9.38), 13.16 (6.72), 13.68 (6.47), 14.18 (6.24), 17.16 (5.16), 17.88 (4.96), 18.50 There are characteristic peaks at (4.79), 19.18(4.62), 20.18(4.40), 21.64(4.10), 22.90(3.88), 26.26(3.39), 28.68(3.11) and 35.90(2.50). The stability investigation data of cadrofloxacin hydrochloride type I crystalline product are shown in Table 1.

Embodiment 2

[0026] Add 2.00 g of cadrofloxacin hydrochloride into water (50 ml), heat to reflux to dissolve, filter, concentrate under reduced pressure to about half the volume to crystallize, slowly cool to room temperature, and filter out the precipitated crystals. The obtained crystals were dried at 40° C. under reduced pressure for 3 hours to obtain 1.72 g of crystals with a yield of 86.0%. Gained sample contains 0.75% moisture; The X-ray diffraction pattern collection of samples of this crystallization and figure 1 Similar to type I crystal.

Embodiment 3

[0028] Add 10.0 g of cadrofloxacin hydrochloride into water (250 ml), heat to reflux to dissolve, filter, concentrate under reduced pressure to about half of the volume, rapidly rinse into absolute ethanol (800 ml), and collect the precipitated solid powder by filtration. The obtained solid was dried under reduced pressure at 40° C. for 5 hours to obtain 8.9 g of the product with a yield of 89.0%. The obtained sample contained 0.72% moisture; from the X-ray diffraction pattern of the crystalline sample, it can be seen that the product was an amorphous powder. The stability investigation data of cadrofloxacin hydrochloride amorphous product are shown in Table 1.

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Abstract

The invention relates to cadrofloxacin hydrochloride-I crystals and a preparation method and applications thereof. The preparation method comprises the following steps: using water which is generally adopted and used as crystallization solvent to crystallize cadrofloxacin hydrochloride solid in any crystal form or amorphous form and obtaining pure cadrofloxacin hydrochloride-I crystals. The cadrofloxacin hydrochloride-I crystals have good crystallization shape, uniform crystal grains and good fluidity; and the crystals have good chemical stability and no residual solvent on the conventional storage condition and can be better used in the preparation of various medicinal dosage forms and the clinical treatments.

Description

technical field [0001] The invention relates to a crystal form of fluoroquinolone antibacterial drugs, in particular to a type I crystal of cadrofloxacin hydrochloride, a preparation method and application thereof. Background technique [0002] The development of effective antibacterial agents is the technology that current researchers focus on. The patent application CN1040977 of Japan Sankyo Co., Ltd. (the corresponding patent application in other countries is US5073556A, EP610958B1) discloses a kind of 4-oxoquinoline-3 -Carboxylic acid derivatives, the specific compound cadrofloxacin in the derivatives has good anti-gram-positive and anti-gram-negative antibacterial activity. Studies have shown that the activity of the fourth-generation fluoroquinolone antibacterial drug katrafloxacin hydrochloride against methicillin-resistant Staphylococcus aureus is 2 to 8 times that of other quinolone antibacterial drugs, and its antibacterial activity is greater than that of toloxaci...

Claims

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Application Information

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IPC IPC(8): C07D401/04A61K31/496A61P31/04
Inventor 孙飘扬陈永江杨宾
Owner SUNCADIA PHARM CO LTD
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