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Crystal forms of flurbiprofen sodium and preparation method thereof

A technology of flurbiprofen sodium and flurbiprofen, which is applied in the pharmaceutical field, can solve problems such as the influence of drug properties, low purity of flurbiprofen sodium, etc., and achieves high liquid phase purity, less types of impurities, and improved stability. Effect

Active Publication Date: 2017-06-30
WUHAN LEADPHARM TECH CO LTD
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Problems solved by technology

[0005] There is no bibliographical report on flurbiprofen sodium crystal structure or related polymorphic forms yet at present, and the medicine of different crystal structure may have different stability, therefore, the present invention has carried out research to the different crystal forms of flurbiprofen sodium
[0006] In addition, in the existing production process for preparing flurbiprofen sodium, the purity of the flurbiprofen sodium product is low, and generally contains impurity A, impurity B, impurity C, impurity D and impurity E, and the limits stipulated by the European Pharmacopoeia of the above impurities are respectively : 0.5%, 0.2%, 0.2%, 0.2%, 0.2%, flurbiprofen sodium contains these impurities, which will have a certain impact on the performance of the drug

Method used

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  • Crystal forms of flurbiprofen sodium and preparation method thereof
  • Crystal forms of flurbiprofen sodium and preparation method thereof
  • Crystal forms of flurbiprofen sodium and preparation method thereof

Examples

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preparation example Construction

[0047] The preparation method of the flurbiprofen sodium crystal form I is as follows: mix and stir flurbiprofen, an antioxidant and a reaction solvent and heat up to 50-100° C. to dissolve, and the addition amount of the antioxidant is flurbiprofen 0.03%~0.3% of the amount, the proportioning of flurbiprofen and the reaction solvent is 1g:2~5ml, then dropwise add NaOH aqueous solution and stir to react for 0.2~2h, the molar feeding ratio of flurbiprofen and sodium hydroxide 1:1~1:1.2, after stopping the reaction, slowly cool to room temperature, then cool down to -5~15°C, stir and crystallize for 0.5~5h, filter, and put the obtained solid in a vacuum degree of 0.08~0.095Mpa, temperature 25~35 After drying at ℃ for 4-6 hours, the crystal form I of flurbiprofen sodium is obtained in the form of white powder. Wherein, the antioxidant is ascorbic acid or sodium sulfite; the reaction solvent is a single solvent water or a mixture of water and an organic solvent, and the organic sol...

Embodiment 1

[0054] This example provides the preparation process of flurbiprofen sodium crystal form I: add 1.221kg flurbiprofen, 3.7g ascorbic acid, 1.832kg water, 1.447kg ethanol to the reaction kettle, heat up to 70-75°C under stirring Dissolve and clear; then start to drop 30% NaOH aqueous solution (containing NaOH 0.200kg); after dropping, keep stirring at the temperature for 1.5h; stop the reaction, slowly cool to room temperature, then cool down to 0-5°C and stir for 2h to crystallize ; Filtration, the obtained solid was kept in a vacuum greater than 0.08Mpa, dried at a temperature of 30-35°C for 5h, and 1.446kg of a white powdery solid was obtained, which was flurbiprofen sodium crystal form Ⅰ. After testing, the yield of flurbiprofen sodium crystal form I in this example is 95.7%, the liquid phase purity is 99.89%, and the water content is 11.89%, and the obtained flurbiprofen sodium crystal form I has high purity and only contains impurities A, impurity A content is 0.06%.

[0...

Embodiment 2

[0067] This example provides the preparation process of flurbiprofen sodium crystal form II: add 1.221kg flurbiprofen and 2.894kg methanol to the reaction kettle, heat up to 65°C under stirring until dissolved; then start to drop 28% methanol Sodium methanol solution 0.965kg; after dripping, keep the temperature and stir for 1.5h; stop the reaction, slowly cool to room temperature, then cool down to 0-5°C and stir for 2h, filter, and keep the vacuum degree of the obtained solid greater than 0.08Mpa, Dry at a temperature of 30-35°C for 5 hours to obtain 1.262 kg of white powdery solid, which is flurbiprofen sodium crystal form II. After testing, the yield of flurbiprofen sodium crystal form II in this embodiment is 94.8%, the liquid phase purity is 99.55%, and the moisture content is 0.15%, and the obtained flurbiprofen sodium crystal form II has high purity, wherein It only contains impurity A and impurity B, the content of impurity A is 0.31%, and the content of impurity B is...

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Abstract

The invention provides three crystal forms of flurbiprofen sodium and a preparation method thereof and specifically relates to three forms, namely, a flurbiprofen sodium crystal form I, a flurbiprofen sodium crystal form II and a flurbiprofen sodium crystal form III of flurbiprofen sodium in a solid state, and structure representation and stability analysis for the three crystal forms. The research data for basic sciences is supplied for researching the stability of the drug which is prepared from the crystal forms. The invention also designs a preparation method for the three crystal forms of flurbiprofen sodium. The method is simple; the obtained product is high in purity; the impurity contents of the flurbiprofen sodium crystal form I and the flurbiprofen sodium crystal form III are both less than 0.1%; and the impurity content of the flurbiprofen sodium crystal form II is less than 0.5%.

Description

technical field [0001] The invention belongs to the technical field of pharmacy, and specifically relates to three forms of flurbiprofen sodium in a solid state: crystal form I, crystal form II and crystal form III, and a preparation method for the three crystal forms. Background technique [0002] Flurbiprofen sodium (as (RS)-2-(2-fluorobiphenyl-4-yl)propionic acid sodium salt or (RS)-2-(2-fluorobiphenyl-4-yl)propionic acid sodium salt Dihydrate) is a phenylpropionic acid non-steroidal anti-inflammatory analgesic. Animal studies have proved that it has analgesic, antipyretic and anti-inflammatory effects, and its mechanism of action is mainly to inhibit the activity of cyclooxygenase (COX), block the synthesis of prostaglandins, and relieve inflammation. The structure of flurbiprofen sodium is as follows: [0003] [0004] The raw material of flurbiprofen sodium is produced by Bausch & Lomb of the United States and was launched in the United States in 1995. Flurbiprof...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/43C07C51/50C07C57/58
CPCC07B2200/13C07C51/43C07C51/50C07C57/58
Inventor 王革吴波徐旻明谢树伟陈蔚江
Owner WUHAN LEADPHARM TECH CO LTD
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