Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

A kind of dapoxetine hydrochloride crystal form and preparation method thereof

A technology of dapoxetine hydrochloride and dapoxetine, applied in chemical instruments and methods, preparation of organic compounds, preparation of aminohydroxy compounds, etc., can solve the problem of low purity and stable crystal form of dapoxetine hydrochloride Generality, affecting the efficacy of the final product, etc., to achieve the effect of easy long-term storage, good temperature and humidity stability, and convenient adaptability

Inactive Publication Date: 2016-01-06
SUZHOU UUGENE BIOPHARMA
View PDF11 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Although the above-mentioned several preparation methods finally synthesized the crystal form of dapoxetine hydrochloride, the purity of the synthesized dapoxetine hydrochloride crystal form was not high, and the stability of the crystal form was average, and these may affect the drug efficacy of the final product

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • A kind of dapoxetine hydrochloride crystal form and preparation method thereof
  • A kind of dapoxetine hydrochloride crystal form and preparation method thereof
  • A kind of dapoxetine hydrochloride crystal form and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Dissolve 10g of dapoxetine in 30mL of ethyl acetate, add 10mL of concentrated hydrochloric acid while stirring, let stand after stirring, separate the layer suspended between the ethyl acetate layer and the water layer, concentrate, and dilute with 20mL of iso After beating with propanol, the crystals were collected by suction filtration and dried to obtain 10.2 g of dapoxetine hydrochloride crystal form. Its purity is 99.79%, chiral purity is 99.51%, and yield is 92%.

Embodiment 2

[0042] Dissolve 10g of dapoxetine in 30mL of methyl acetate, add 10mL of concentrated hydrochloric acid while stirring, let it stand after stirring, separate the layer suspended between the ethyl acetate layer and the water layer, concentrate, and dilute with 20mL of normal After beating with butanol, the crystals were collected by suction filtration and dried to obtain 10.5 g of dapoxetine hydrochloride crystal form. Its purity is 99.31%, chiral purity is 99.10%, and yield is 94.7%.

Embodiment 3

[0044] Take 10g of dapoxetine and dissolve it in 30mL of isopropyl acetate to form a reaction solution, feed dry hydrogen chloride gas into the reaction solution while stirring in an ice-salt bath until no solid is precipitated, collect crystals by suction filtration, and dry to obtain 9.9 g of dapoxetine hydrochloride crystal form. The yield is 89.2%, the purity is 99.12%, and the chiral purity is 99.01%.

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

PropertyMeasurementUnit
melting pointaaaaaaaaaa
Login to View More

Abstract

The invention relates to a dapoxetine hydrochloride crystal form and a preparation method thereof and belongs to the technical field of pharmaceutical synthesis. The dapoxetine hydrochloride crystal form uses Cu-Ka radiation and employs 2 theta angle to express characteristic peaks of X-ray powder diffraction at 6.82+ / -0.2, 8.90+ / -0.2, 13.69+ / -0.2, 15.03+ / -0.2, 16.04+ / -0.2, 17.78+ / -0.2, 18.82+ / -0.2, 20.61+ / -0.2, 21.65+ / -0.2, 22.26+ / -0.2, 22.66+ / -0.2, 25.23+ / -0.2, 27.61+ / -0.2, 28.89+ / -0.2; the DSC scan shows a first endothermic peak between 55-85 DEG C and a second endothermic peak between 150-200 DEG C. The invention provides a method for preparing the crystal form. The dapoxetine hydrochloride crystal form has good appearance, good temperature and humidity stability, high melting point and high purity, and is convenient for long-term storage.

Description

technical field [0001] The invention relates to a dapoxetine hydrochloride crystal form and a preparation method thereof, belonging to the technical field of drug synthesis. Background technique [0002] Dapoxetine hydrochloride (dapoxetinehydrochloride), is a selective serotonin reuptake inhibitor (SSRI), developed by Eli Lilly (Eli Lilly), listed in Europe in 2009, the trade name is Priligy, used for Treatment of premature ejaculation (PE) in men. The drug has a short half-life, few adverse reactions, and significant effects. It is the world's first oral prescription drug approved for the treatment of PE, and the world's first oral drug for this indication. It was approved by ThomsonReuters in 2009 The quarterly report on major progress in global drug development in the first quarter is listed as one of the five most promising drugs that have been marketed or are under approval. [0003] Dapoxetine hydrochloride, chemical name: (S)-(+)-(N,N-dimethylamino)-3-(naphthyl-1-o...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Patents(China)
IPC IPC(8): C07C217/48C07C213/10
Inventor 胡凡邵长坤李胜陈冠元王伸勇王晓俊胡长春
Owner SUZHOU UUGENE BIOPHARMA
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com