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Preparation method of flucloxacillin sodium crystal form III

A technology of flucloxacillin sodium and crystal form, applied in the direction of organic chemistry, etc., can solve problems such as unstable solubility properties

Active Publication Date: 2013-09-11
GUILIN UNIVERSITY OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Flucloxacillin sodium API is analyzed as a mixture of amorphous and unknown crystal forms, and its solubility is unstable

Method used

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  • Preparation method of flucloxacillin sodium crystal form III
  • Preparation method of flucloxacillin sodium crystal form III
  • Preparation method of flucloxacillin sodium crystal form III

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0057] 1. Preparation of flucloxacillin sodium crystal form I:

[0058] Add 1.0 g of flucloxacillin sodium bulk drug and 17 mL of isopropanol into a 50 mL three-necked flask, stir with magnetic force at a stirring speed of 20 r / min. After heating at 50-55°C for 0.5h, filter while it is hot, collect the filtrate, cool and crystallize at room temperature, collect the crystals after precipitation and dry at a constant temperature of 50°C, dry for 12 hours and store in a desiccator sealed at room temperature.

[0059] 2. Confirmation of flucloxacillin sodium crystal form I:

[0060] 1. UV spectrophotometry:

[0061] Use phosphate buffer solution with pH=6.8 to configure 1g / L flucloxacillin sodium standard and flucloxacillin sodium crystal form I solution, quartz cuvette, and phosphate buffer solution with pH=6.8 as blank reagent.

[0062] Operating conditions:

[0063] Detector: UV-2450 ultraviolet spectrophotometer

[0064] As a result, the crystalline form I of flucloxacil...

Embodiment 2

[0084] 1. Preparation of flucloxacillin sodium crystal form II:

[0085] Add 2.0 g of flucloxacillin sodium bulk drug and 20 mL of ethanol into a 50 mL three-necked flask, and stir magnetically at a stirring speed of 20 r / min. After heating under boiling conditions for 0.5h, filter while it is hot, slowly cool and crystallize, collect the crystals after precipitation and dry at a constant temperature of 50°C, dry for 12 hours and store in a desiccator sealed at room temperature.

[0086] 2. Confirmation of flucloxacillin sodium crystal form II:

[0087] 1. UV spectrophotometry:

[0088] Use phosphate buffer solution with pH=6.8 to configure 1g / L flucloxacillin sodium standard and flucloxacillin sodium crystal form II solution, quartz cuvette, and phosphate buffer solution with pH=6.8 as blank reagent.

[0089] Operating conditions:

[0090] Detector: UV-2450 ultraviolet spectrophotometer

[0091]As a result, the crystalline form II of flucloxacillin sodium obtained a...

Embodiment 3

[0111] 1. Preparation of flucloxacillin sodium crystal form III:

[0112] Add 1.0 g of flucloxacillin sodium bulk drug and 13 mL of acetone into a 50 mL three-necked flask, stir with magnetic force at a stirring speed of 20 r / min. After heating under boiling conditions for 0.5h, filter while it is hot, cool and crystallize at a lower temperature (5-15°C), collect the crystals after precipitation and dry at a constant temperature of 50°C, dry for 12 hours and seal them in a desiccator at room temperature.

[0113] 2. Confirmation of flucloxacillin sodium crystal form III:

[0114] 1. UV spectrophotometry:

[0115] Use phosphate buffer solution with pH=6.8 to configure 1g / L flucloxacillin sodium standard and flucloxacillin sodium crystal form III solution, quartz cuvette, and phosphate buffer solution with pH=6.8 as blank reagent.

[0116] Operating conditions:

[0117] Detector: UV-2450 ultraviolet spectrophotometer

[0118] As a result, the crystal form III of flucloxa...

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Abstract

The invention discloses a preparation method of a flucloxacillin sodium crystal form III. The preparation method comprises the following steps of: dissolving 1.0g of flucloxacillin sodium raw material medicines in 13mL of acetone; magnetically stirring; heating for 0.5 h in a boiling condition, and then filtering while hot; performing cooling crystallization at 5-15 DEG C; collecting crystals after the crystallization, and drying at a constant temperature of 50 DEG C; and drying for 12 hours, and air-tightly storing in a drier at a normal temperature. The flucloxacillin sodium crystal form III prepared by the preparation method disclosed by the invention is high in solubility in a neutral environment (with a pH of 6.8), thus showing high bioavailability.

Description

[0001] The application date of this case is June 17, 2011, the application number is 2011101650164, and the name of the invention is: a divisional application for the preparation method of flucloxacillin sodium amorphous and three polymorphs. technical field [0002] The invention relates to a preparation method of flucloxacillin sodium amorphous crystal form and three polymorphic forms. Background technique [0003] Flucloxacillin sodium [chemical name: (2S, 5R, 6R) -6-[[3-(2-chloro-6-fluorophenyl)-5-methyl-1,2-oxazole-4-formyl ]amino]-3,3-dimethyl-7-oxo-4-thia-1-azabicyclo[3.2.0]heptane-2-carboxylic acid sodium salt] known as a semi-synthetic penicillin antibacterial medicine. The same drug uses different solvents, and the crystallization process makes the resulting crystals have different spatial structures, which we call drug polymorphism. Drug polymorphism is generally considered to have four types: conformational polymorphism, configuration polymorphism, color polymo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D499/76
Inventor 刘峥周肖寅王苗苗
Owner GUILIN UNIVERSITY OF TECHNOLOGY
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