Preparation method of flucloxacillin sodium crystal form II

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: 2015-05-20
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 II
  • Preparation method of flucloxacillin sodium crystal form II
  • Preparation method of flucloxacillin sodium crystal form II

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 to a 50 mL three-necked flask, stir magnetically, and stir at a speed of 20 r / min. After heating at 50-55°C for 0.5h, filter while hot, collect the filtrate, cool at room temperature for crystallization, collect crystals after precipitation, and dry at 50°C at a constant temperature. After drying for 12 hours, keep in a desiccator at room temperature.

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

[0060] 1. Ultraviolet spectrophotometry:

[0061] Phosphate buffer solution with pH=6.8 was used to prepare 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 flucloxacillin...

Embodiment 2

[0083] 1. Preparation of flucloxacillin sodium crystal form II:

[0084] Add 2.0 g of flucloxacillin sodium bulk drug and 20 mL of ethanol to a 50 mL three-necked flask, stir magnetically, and stir at a speed of 20 r / min. After heating for 0.5h under boiling conditions, filter while hot, slowly cool for crystallization, collect crystals after precipitation, and dry them at a constant temperature of 50°C, and store them in a desiccator at room temperature after drying for 12 hours.

[0085] 2. Confirmation of the crystal form II of flucloxacillin sodium:

[0086] 1. Ultraviolet spectrophotometry:

[0087] Phosphate buffer solution with pH=6.8 was used to prepare 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.

[0088] Operating Conditions:

[0089] Detector: UV-2450 Ultraviolet Spectrophotometer

[0090] As a result, the crystalline form II of flucloxaci...

Embodiment 3

[0109] 1. Preparation of flucloxacillin sodium crystal form III:

[0110] 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.

[0111] 2. Confirmation of flucloxacillin sodium crystal form III:

[0112] 1. UV spectrophotometry:

[0113] 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.

[0114] Operating conditions:

[0115] Detector: UV-2450 ultraviolet spectrophotometer

[0116] 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 II. The preparation method comprises the following steps of: dissolving 2.0g of flucloxacillin sodium raw material medicines in 20mL of ethanol; magnetically stirring; heating for 0.5 hour in a boiling condition, and then filtering while hot; slowly performing cooling crystallization; 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 II 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 Patents(China)
IPC IPC(8): C07D499/76C07D499/18
Inventor 刘峥周肖寅王苗苗
Owner GUILIN UNIVERSITY OF TECHNOLOGY
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