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Preparation method of flurbiprofen axetil

The technology of flurbiprofen axetil and flurbiprofen axetil is applied in the field of preparation of pharmaceutical grade flurbiprofen axetil, and can solve the problems of complicated preparation operation, unfavorable unification of quality standards of preparation raw materials and product, increase of preparation production cost and the like.

Active Publication Date: 2013-08-21
WUHAN DOCAN PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Therefore, it is necessary to carry out additional purification to flurbiprofen axetil raw material before being used in the preparation, and this process makes the pre-preparation operation more loaded down with trivial details, has increased preparation production cost greatly, is difficult to realize large-scale production and popularization and application, is also unfavorable for each preparation Unification of raw material product quality standards

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  • Preparation method of flurbiprofen axetil
  • Preparation method of flurbiprofen axetil
  • Preparation method of flurbiprofen axetil

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preparation example Construction

[0020] The invention provides a kind of preparation method of flurbiprofen axetil, comprising the following steps:

[0021] (a) reacting flurbiprofen and bromoethyl acetate in the presence of a catalyst and a solvent;

[0022] (b) washing the product of the reaction to separate the oil;

[0023] (c) Distill the oil under reduced pressure and collect fractions at 173-175°C / 0.8mmHg;

[0024] (d) dissolving the collected fractions in an organic solvent, washing and drying; and

[0025] (e) Removing the organic solvent.

[0026] Flurbiprofen axetil of the present invention refers to (±) 2-(2-fluoro-4-biphenyl)propionic acid-1-acetoxy ethyl ester, and its structural formula is as follows:

[0027]

[0028] In one embodiment of the present invention, the method further comprises the steps of dissolving the separated oil in an organic solvent after step (b), washing (such as washing with water), drying, and removing the organic solvent (b-1 ).

[0029] In one embodiment of th...

Embodiment 1

[0085] Add 12.2g (0.05mol) flurbiprofen (purchased from Kangning Chemical Co., Ltd., Sanmen County, Zhejiang Province) and about 100ml of newly distilled acetone in the reaction flask, mix, add 5.9g (0.07mol) sodium acetate; The reaction mixture was cooled to 5-10°C with ice water, and 11.7g (0.07mol) of bromoethyl acetate (purchased from Quanxi Chemical Factory, Huixian City, Henan Province) was added dropwise. The reaction was stirred for 5h.

[0086] After the reaction was completed, the insoluble matter was filtered off, and about 20 ml of 2.5% (w / v) sodium carbonate aqueous solution was added to the filtrate, and the oily substance in the lower layer was separated after standing. The oil in the lower layer was dissolved in about 100ml of n-hexane, washed with about 30ml of water, and dried by adding anhydrous magnesium sulfate; the desiccant was filtered off, and the n-hexane was evaporated under reduced pressure.

[0087] The obtained product was distilled under reduced...

Embodiment 2

[0091] Add 12.2g (0.05mol) flurbiprofen (purchased from Kangning Chemical Co., Ltd., Sanmen County, Zhejiang Province) and about 100ml of newly distilled ethyl acetate in the reaction flask, mix well, add 7.6g (0.02mol) dodecyl Sodium Phosphate Hydrate. The reaction mixture was cooled to 5-10°C with ice water, and 11.7g (0.07mol) of bromoethyl acetate (purchased from Quanxi Chemical Factory, Huixian City, Henan Province) was added dropwise. The reaction was stirred for 6h.

[0092] After the reaction was completed, the insolubles were filtered off, and about 15ml of 4% (w / v) sodium carbonate aqueous solution was added to the filtrate, and the lower layer oil was separated after standing. The oil in the lower layer was dissolved in about 100ml of n-hexane, washed with about 30ml of water, and dried by adding anhydrous magnesium sulfate; the desiccant was filtered off, and the n-hexane was evaporated under reduced pressure.

[0093] The obtained product was distilled under red...

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Abstract

The invention relates to a preparation method of flurbiprofen axetil. The method comprises the following steps: carrying out a reaction between flurbiprofen and bromoethyl acetate in the presence of a catalyst and a solvent; washing reaction products and separating grease; carrying out underpressure distillation; dissolving a fraction in an organic solvent, washing and drying; and removing the solvent. Purity of flurbiprofen axetil prepared by the method can reach more than 99.0%.

Description

technical field [0001] The invention relates to the technical field of pharmacy, in particular to a preparation method of pharmaceutical grade flurbiprofen axetil. Background technique [0002] Flurbiprofen axetil (Flurbiprofen Axetil) is a non-steroidal anti-inflammatory drug, and its commonly used preparation is flurbiprofen axetil (lipid microspheres) injection, which is a targeted drug delivery preparation and is used clinically in surgery and cancer pain relief. [0003] In order to reduce the unnecessary side effects brought by the impurities in the raw materials of flurbiprofen axetil, the flurbiprofen axetil as the raw material used in common preparations requires high purity. At present, the commercially available flurbiprofen axetil is of industrial grade, and its purity cannot reach 99.0%, which is not suitable for direct use in the preparation of pharmaceutical preparations, especially injections. Therefore, it is necessary to carry out additional purification ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/65C07C67/11A61K31/222A61P29/00
Inventor 陈邦银张文军
Owner WUHAN DOCAN PHARMA
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