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

Bilastine crystal and preparation method thereof

A crystal form, benzodiimazole technology, applied in the field of medicine, achieves good stability and is not easy to crystallize.

Inactive Publication Date: 2013-07-24
BEIJING VENTUREPHARM BIOTECH
View PDF3 Cites 12 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The patent only gives the crystal form The unit cell data and infrared data, the crystallization solvent used is isopropanol, n-butanol, acetone, DMF, DMSO, THF, acetonitrile or their mixture

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
  • Bilastine crystal and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] 1.0 g of 4-[2-[1-(2-ethoxyethyl)-1H-benzodiimazol-2-yl]-1-piperidinyl]ethyl]-α,α-dimethyl Phenylacetic acid was added to 8ml of methanol, heated to dissolve, refluxed for one hour, naturally cooled and crystallized, filtered, and dried in vacuum at 50°C for 10 hours to obtain 0.72 grams of 4-[2-[1-(2-ethoxyethyl) -1H-Benzodeimazol-2-yl]-1-piperidinyl]ethyl]-α,α-Dimethylphenylacetic acid new crystal form, the yield is 72%, and the measured melting point is 197-200°C .

Embodiment 2

[0018] 2.0 g of 4-[2-[1-(2-ethoxyethyl)-1H-benzodiimazol-2-yl]-1-piperidinyl]ethyl]-α,α-dimethyl Add phenylacetic acid to 16ml of toluene, heat to dissolve, keep the temperature at about 70°C, keep it warm for one hour, cool and crystallize naturally, filter, and dry in vacuum at 50°C for 10 hours to obtain 1.5 grams of 4-[2-[1-(2 -Ethoxyethyl)-1H-benzodiimazol-2-yl]-1-piperidinyl]ethyl]-α,α-Dimethylphenylacetic acid new crystal form, yield 75%, measured The melting point is 197.5-200.2°C.

Embodiment 3

[0020] 1.5 g of 4-[2-[1-(2-ethoxyethyl)-1H-benzodiimazol-2-yl]-1-piperidinyl]ethyl]-α,α-dimethyl Add phenylacetic acid to 14ml of ethyl acetate, heat to dissolve, keep the temperature at about 65°C, keep it warm for one hour, cool and crystallize naturally, filter, and dry in vacuum at 50°C for 10 hours to obtain 1.0 g of 4-[2-[1- New crystal form of (2-ethoxyethyl)-1H-benzodiimazol-2-yl]-1-piperidinyl]ethyl]-α,α-dimethylphenylacetic acid, yield 66.7% , and the measured melting point is 197.5-199.8°C.

[0021] attached figure 1 X-powder diffraction pattern of bilastine crystal form

[0022] degree 2θ d-spacing Relative Strength(%) 9.2717 9.54 69.73 10.9004 8.11 35.37 12.7461 6.94 53.88 15.6617 5.65 45.34 17.6890 5.01 100.00 18.3202 4.84 64.71 20.0376 4.43 77.25 21.9021 4.05 52.89 27.3518 3.26 26.65

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
Melting pointaaaaaaaaaa
Login to View More

Abstract

The invention belongs to the technical field of medicines, and particularly relates to 4-[2-[1-(2-ethoxy ethyl)-1H-benzodimazole-2-based]-1-piperidyl] ethyl]-alpha, alpha-methyl phenylpropionic acid (bilastine) crystal and a preparation method thereof. According to the method, bilastine is added into an organic solvent, heated to dissolve and then cooled to crystallize to obtain the bilastine crystal.

Description

technical field [0001] The invention belongs to the technical field of medicine and relates to a kind of 4-[2-[1-(2-ethoxyethyl)-1H-benzodiimazol-2-yl]-1-piperidinyl]ethyl] -α,α-Dimethylphenylacetic acid (bilastine) crystal form and preparation method. Background technique [0002] Bilastine, chemical name 4-[2-[1-(2-ethoxyethyl)-1H-benzodiimazol-2-yl]-1-piperidinyl]ethyl]-α, α-Dimethylphenylacetic acid, whose structure is shown in the following formula, is a kind of H 1 Receptor antagonists, not only for H 1 Receptor has antagonistic effect, and also inhibits the release of histamine and L-4 from inflammatory mediators, so it does not have the sedative effect and cardiotoxicity of commonly used antihistamines, and is mainly used clinically for the treatment of allergic rhinitis and chronic idiopathic rhinitis hives. First launched in Ireland in 2011. [0003] [0004] In US Patent No. 5877187, the preparation method of bilastine was first mentioned, but the patent ...

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
IPC IPC(8): C07D401/04A61K31/454A61P37/08A61P11/02A61P17/00
Inventor 侯艳超马苏峰闫起强
Owner BEIJING VENTUREPHARM BIOTECH
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