Dapoxetine hydrochlorate crystal form A and preparation method thereof

A technology of dapoxetine hydrochloride and crystal form, applied in the field of organic chemistry

Inactive Publication Date: 2013-06-05
CHONGQING PHARMA RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The preparation method of dapoxetine hydrochloride has been disclosed in EP0288188, WO2008035358, US5292962, CN101012147, CN1821212, CN101875666 and other patents, but its crystal form and crystal form preparation method No literature report

Method used

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  • Dapoxetine hydrochlorate crystal form A and preparation method thereof
  • Dapoxetine hydrochlorate crystal form A and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] Preparation of Dapoxetine Hydrochloride Form A

[0050] Dissolve 2g of dapoxetine hydrochloride solid in 20ml of isopropanol, heat to reflux to dissolve and clarify, let stand and cool to room temperature, add to 150ml of cyclohexane under stirring, after addition, stir at room temperature for about 50min, filter, and The filter cake was dried under vacuum at 40-50°C to obtain dapoxetine hydrochloride Form A, whose X-ray powder diffraction pattern is shown in figure 1 , the main test data values ​​are listed in the following table (list the test data with relative strength greater than or equal to 4%).

[0051] 2θ angle (°) measured value d(?) Measured value Relative Strength(%) 8.88540 9.94422 14 14.3676 6.15980 30 15.0761 5.87188 39 16.3200 5.42702 20 16.6400 5.32337 14 16.9600 5.22364 4 17.7987 4.97934 10 18.8786 4.69688 57 19.2600 4.60472 8 20.6811 4.29140 25 21.2000 4.18752 5 21.76...

Embodiment 2

[0053] Preparation of Dapoxetine Hydrochloride Form A

[0054] Dissolve 2g of dapoxetine hydrochloride solid in 16ml of absolute ethanol, heat to reflux to dissolve and clarify, filter, add the filtrate to 100ml of ether with stirring, after the addition is complete, stir at room temperature for about 30min, then cool to 5°C and stir for about 30min , filtered, and the filter cake was dried under vacuum at 40~50°C to obtain dapoxetine hydrochloride crystal form A, and the X-ray powder diffraction pattern was within the error range and figure 1 unanimous.

Embodiment 3

[0056] Dissolve 5g of dapoxetine hydrochloride sample in 50ml of methanol, heat to reflux to dissolve and clarify, add 200ml of n-pentane / methyl acetate (volume ratio 3:1) mixture to the reaction solution, after the addition is complete, cool to 0 ~5°C for static crystallization for about 60 minutes, filter, and vacuum-dry the filter cake at 50~60°C to obtain dapoxetine hydrochloride crystal form A, whose X-ray powder diffraction pattern is within the error range and figure 1 unanimous.

[0057]

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PUM

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Abstract

The invention relates to a crystal form A of dapoxetine hydrochlorate which is a drug for treating male premature ejaculation, and a preparation method thereof; the crystal form A is characterized in that the crystal form A has characteristic diffraction peaks corresponding to positions with 2theta values of about 8.9 degrees, 14.4 degrees, 15.1 degrees, 16.3 degrees, 16.6 degrees, 18.9 degrees, 20.7 degrees, 22.7 degrees, 23.8 degrees, 25.3 degrees, 29.0 degrees, and 29.5 degrees on an X-ray powder diffraction pattern, and the new crystal form has the characteristics of high purity, good stability, and the like.

Description

technical field : [0001] The present invention relates to the fields of organic chemistry and pharmacy, in particular to a new crystal form A of dapoxetine hydrochloride, a drug for treating premature ejaculation in men, and a preparation method thereof, a pharmaceutical composition containing the new crystal form, and the new crystal form Application in the manufacture of medicines for treating premature ejaculation in men. technical background: [0002] Dapoxetine Hydrochloride, chemical name S-(+)-N,N-dimethyl-1-phenyl-3-(1-naphthyloxy)propylamine hydrochloride (S-(+) -N,N-dimethyl-3-(naphthalene-1-yloxy)-1- [0003] phenylpropan-1-amine Hydrochloride), the chemical structural formula is as shown in (I), and can be prepared according to the method disclosed in the patent EP0288188. [0004] [0005] Dapoxetine hydrochloride is a selective serotonin reuptake inhibitor (SSRI) for the treatment of premature ejaculation and erectile dysfunction in adult males, and it i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C217/48C07C213/10A61K31/138A61P15/08A61P15/00
Inventor 邹益品吴科罗杰蔡中文叶文润樊斌
Owner CHONGQING PHARMA RES INST
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