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Refining method for avanafil

A technology of avanafil and refining method, which is applied in the field of medicine, can solve the problems of poor dissolution effect and insufficient dissolution rate, and achieve the effects of high purity and yield, easy operation and good economic benefits

Active Publication Date: 2017-01-18
SHANDONG CHENGCHUANG PHARMA R&D
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Moreover, the applicant found that the dissolution effect of the bulk drug prepared by this method was not good when made into tablets, and the dissolution rate was far inferior to that of the original drug.

Method used

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  • Refining method for avanafil

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] At room temperature, 20 g of crude avanafil with a purity of 98.5% (as determined by HPLC) was added to a mixed solvent of 280 mL of ethyl acetate and 140 mL of absolute ethanol, stirred evenly, heated to reflux, and after the solid was completely dissolved, let it stand naturally After cooling down to 40°C, start stirring, and cool down to 10°C in an ice bath. Incubate for 1 hour, filter, collect the filter cake, and dry under vacuum (-0.09Mpa) at 40-50°C for 8 hours to obtain 16 g of avanafil with a purity of 99.91% (as determined by HPLC). Yield: 80%.

[0032] Solvent residue: ethyl acetate, 0.08%, ethanol 0.10% (as determined by GC), particle size: ≤30 μm.

Embodiment 2

[0034] At room temperature, 50 g of avanafil crude product with a purity of 98.5% (as determined by HPLC) was added to a mixed solvent of 300 mL of methanol and 600 mL of isopropyl ether, after stirring evenly, it was heated to reflux, and after the solid was completely dissolved, it was allowed to stand and naturally cooled to 30°C, start stirring, cool down to 0°C in an ice bath, keep warm for 3 hours, filter, collect the filter cake, and dry under vacuum (-0.09Mpa) at 40-50°C for 8 hours to obtain 41g of avanafil with a purity of 99.90% (as determined by HPLC ). Yield: 82%.

[0035] Solvent residue: no detection of isopropyl ether, 0.13% methanol (measured by GC), particle size: ≤30 μm.

Embodiment 3

[0037] At room temperature, add 100 g of crude avanafil with a purity of 98.5% (as determined by HPLC) into a mixed solvent of 100 mL of dimethyl sulfoxide and 500 mL of ethyl acetate, stir and heat to reflux. After the solid is completely dissolved, cool down naturally To 20°C, start stirring, slowly cool down to -10°C in an ice bath, keep warm for 2 hours, filter, collect filter cake, and dry under vacuum (-0.09Mpa) at 75-80°C for 12 hours to obtain 83.5g of avanafil with a purity of 99.93% (HPLC determination). Yield: 83.5%.

[0038] Solvent residues: 0.15% dimethyl sulfoxide, 0.19% ethyl acetate (measured by GC), particle size: ≤30 μm.

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Abstract

The invention discloses a refining method for avanafil. An avanafil bulk drug prepared by using the refining method has a particle size of no more than 30 [mu]m; so in the process of drying, an organic solvent can be easily volatilized and solvent residues are low in amount. The refining method comprises the following concrete steps: adding a crude avanafil product into an organic solvent and carrying out heating to a reflux state; after complete dissolving of solids, carrying out standing for cooling to 40 to 20 DEC C; then carrying out stirring for cooling to 10 to -10 DEG C and maintaining the temperature for 1 to 3 h; carrying out filtering; and subjecting a filter cake obtained in the previous step to vacuum drying. The organic solvent is a combination of two solvents, wherein one solvent is a strongly polar solvent and the other solvent is a moderately polar or non-polar solvent.

Description

technical field [0001] The invention relates to a refining method, in particular to a refining method of avanafil. It belongs to the field of medical technology. Background technique [0002] Avanafil (Avanafil) is authorized by Mitsubishi Tanabe Pharmaceutical Co., Ltd. of Japan and developed by American Vefors Pharmaceuticals for the treatment of male erectile dysfunction. Avanafil is an oral, fast-acting, highly selective phosphodiesterase-5 (PDE-5) inhibitor, which can inhibit the metabolism of cyclic guanosine monophosphate in the body, thereby enhancing the relaxation of smooth muscle and reducing blood flow in the penis. Increased flow, which in turn aids in an erection. Its chemical structural formula is as follows: [0003] [0004] Chinese patent application CN103819460A discloses a process for refining avanafil, the method includes the following steps: [0005] 1) Add the crude product of avanafil into a reaction kettle containing dichloromethane, stir and ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D403/14
CPCC07D403/14
Inventor 李广运王敬美吕志涛
Owner SHANDONG CHENGCHUANG PHARMA R&D
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