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Crystal and amorphous substance of dapoxetine hydrochloride and preparation method thereof

A technology of dapoxetine hydrochloride and dapoxetine, which is applied in the preparation of organic compounds, the preparation of aminohydroxy compounds, and organic chemical methods, etc., can solve the problems of unobtained product dapoxetine hydrochloride and the like

Active Publication Date: 2013-06-05
XIAMEN FUMAN PHARMA +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The preparation of the hydrochloride of dapoxetine is also described in the patent CN1709859, but no characterization is made to it, and the experiment is repeated according to this method, and the product dapoxetine hydrochloride is not obtained

Method used

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  • Crystal and amorphous substance of dapoxetine hydrochloride and preparation method thereof
  • Crystal and amorphous substance of dapoxetine hydrochloride and preparation method thereof
  • Crystal and amorphous substance of dapoxetine hydrochloride and preparation method thereof

Examples

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preparation example Construction

[0033] Reference Example A Preparation of Crystal Form Dapoxetine Hydrochloride

[0034] Weigh 916mg of dapoxetine into a container, add 15ml of ethyl acetate at room temperature, stir until the solid is completely dissolved, filter out insoluble impurities, then pass dry hydrogen chloride gas into it, stir for 2 hours at room temperature, and precipitate , and filtered to obtain 620 mg of white powder, which is the A crystal form of dapoxetine hydrochloride. Its XRPD pattern and DSC pattern see image 3 and Figure 4 . The 2θ value of its XRPD pattern is 6.33, 8.92, 14.42, 15.11, 16.34, 16.65, 16.95, 17.84, 18.93, 19.18, 20.70, 20.93, 21.16, 22.73, 23.82, 25.34, 26.66, 27.80, 29.03, 29.25 , 33.03, 33.67, 34.24, 36.05, 37.32, 38.88, 41.68, 43.45, 44.58, there are diffraction peaks, and the error range of the 2θ value is ±0.2; the DSC spectrum has an endothermic peak at 177±5°C.

Embodiment 1B

[0035] The preparation of embodiment 1B crystal form dapoxetine hydrochloride

[0036] Weigh 916mg of dapoxetine into a container, add 15ml of dichloromethane, stir at room temperature until the solid is completely dissolved, filter off the insoluble matter, then slowly drop into 1.5ml of a saturated solution of hydrogen chloride in dichloromethane, stir at room temperature for 2h, there is precipitation Precipitate, lower the temperature to 5° C., filter, and vacuum-dry to obtain 800 mg of white powder, which is Dapoxetine Hydrochloride in Form B of the present invention. Its XRPD pattern and single crystal structure diagram are shown in figure 1 and figure 2 . In its XRPD pattern, the radiation source is CuKα 1 , at the diffraction angle 2θ values ​​are 6.29, 8.84, 14.33, 15.06, 16.28, 16.38, 16.61, 16.89, 17.78, 18.87, 20.62, 20.76, 21.10, 21.82, 22.69, 23.78, 25.30, 26.66, 27.75, 28.976, , 30.19, 31.22, 31.54, 32.11, 32.96, 33.57, 34.91, 35.25, 35.92, 38.88, 41.64, 44.5...

Embodiment 2

[0037] The preparation of embodiment 2 amorphous dapoxetine hydrochloride

[0038] Dissolve 500 mg of dapoxetine hydrochloride (form B obtained in Example 1) in 20 mL of methanol, filter out the insoluble matter after complete dissolution, quickly remove the solvent by rotary evaporation, and obtain a white solid after vacuum drying, which is the amorphous compound of the present invention. Form Dapoxetine hydrochloride. Its XRPD spectrum and DSC spectrum are shown in Figure 5 and Figure 6 .

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Abstract

The invention discloses a crystal of dapoxetine hydrochloride, amorphous substance of the dapoxetine hydrochloride and a preparation method of the crystal and the amorphous substance of the dapoxetine hydrochloride. The stability of the crystal is better than that of crystal forms in the prior art, and the solubility of the amorphous substance is obvious higher than that of existing dapoxetine hydrochloride.

Description

technical field [0001] The invention specifically relates to a crystal, an amorphous substance of dapoxetine hydrochloride and a preparation method thereof. Background technique [0002] The chemical name of Dapoxetine is (+) N, N-dimethyl-1-phenyl-3-(1-naphthyloxy) propylamine, which is a selective serotonin reuptake inhibitor (SSRI), With a short half-life, it is useful in the treatment of depression and related affective disorders. February 2009 as a drug for the treatment of male premature ejaculation (Prilig TM ) was approved for marketing in Europe, which is the world's first oral drug for this indication, and was listed as the five most important drugs that have been marketed or are being approved by Thomson Reuters in the first quarter of 2009. One of the promising drugs. [0003] The original manufacturer of dapoxetine is Eli Lili Company of the United States, and its original patent EP 0288188 describes the preparation method of dapoxetine. [0004] Patents US ...

Claims

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Application Information

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IPC IPC(8): C07C217/48C07C213/08
CPCA61K31/138C07B2200/13C07C213/08C07C217/48
Inventor 任国宾任秉钧齐明辉乐云峰洪鸣凰曹国斌陈金瑶
Owner XIAMEN FUMAN PHARMA
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