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

Method for separating chiral compound by using molecular sieves

A chiral compound and separation method technology, applied in the field of pharmaceutical synthesis and organic compound synthesis and preparation, can solve the problems of difficult high-purity products, large amount of solvents, low production volume, etc., achieve rapid and effective separation, shorten production cycle, and reduce production pollution small effect

Active Publication Date: 2013-02-27
CP PHARMA QINGDAO CO LTD
View PDF12 Cites 1 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

WO94 / 027988 and WO2007140608 introduced two preparation methods of esomeprazole sodium salt. The defect of these two methods is that a large amount of solvents are used in the preparation process, and the product purity cannot be guaranteed
[0008] In summary, the existing chiral compound separation technology methods have certain limitations, resulting in low production capacity, long cycle, low yield, and it is difficult to obtain high-purity products.

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
  • Method for separating chiral compound by using molecular sieves
  • Method for separating chiral compound by using molecular sieves

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Get molecular sieve zeolite (molecular formula: 4K 2 O·2Na 2 O·6Al 2 o 3 12SiO2 2 27H 2 O, the effective pore diameter is about 0.3nm) placed in glacial acetic acid, take 1α, 25-(OH) 2 -cycling-VD 3 The sample was stirred and dissolved in glacial acetic acid at 30°C, continued to stir for 15 minutes, sealed and stood for 1 hour, extracted three times with ethyl acetate, combined and concentrated the extracts, dissolved in absolute ethanol, and dissolved sodium hydroxide in Add methanol dropwise, stir at room temperature for 1 hour, extract three times with ethyl acetate after the reaction is complete, combine the extracts and wash with saturated aqueous sodium chloride until neutral, dry, filter, evaporate the filtrate to dryness and dissolve in ethyl acetate Add n-pentane to the ester, cool to room temperature and let stand for 12 hours. Acicular crystals are precipitated. The crystals are collected by filtration and vacuum-dried to obtain calcitriol with a purit...

Embodiment 2

[0020] Get molecular sieve zeolite (molecular formula: 2Na 2 O·2Al 2 o 3 4SiO2 2 9H 2 O, the effective pore diameter is about 0.4nm) placed in glacial acetic acid, take 1α, 25-(OH) 2 -cycling-VD 3 The sample was stirred and dissolved in glacial acetic acid at 30°C, continued to stir for 15 minutes, sealed and stood for 1 hour, extracted three times with ethyl acetate, combined and concentrated the extracts, dissolved in absolute ethanol, and dissolved sodium hydroxide in Add methanol dropwise, stir at room temperature for 1 hour, extract three times with ethyl acetate after the reaction is complete, combine the extracts and wash with saturated aqueous sodium chloride until neutral, dry, filter, evaporate the filtrate to dryness and dissolve in ethyl acetate Add n-pentane to the ester, cool to room temperature and let it stand for 12 hours. Acicular crystals precipitate out. The crystals are collected by filtration and vacuum-dried to obtain calcitriol with a purity of 99....

Embodiment 3

[0026] Get molecular sieve zeolite (molecular formula: 4K 2 O·2Na 2 O·6Al 2 o 3 12SiO2 2 27H 2 O, the effective pore diameter is about 0.3nm) placed in glacial acetic acid, take 1α-OH-3,5-cyclo-VD 3 The sample was stirred and dissolved in glacial acetic acid under the condition of 55°C, continued to stir for 25 minutes, sealed and stood for 1 hour, the reaction solution was neutralized with saturated aqueous sodium bicarbonate solution, the pH value was adjusted to 8.0, extracted three times with ether, and the ether layer was washed with water To neutrality, dehydrate with anhydrous magnesium sulfate, filter and concentrate, dissolve in absolute ethanol, and dissolve sodium hydroxide in methanol, add it dropwise, stir at room temperature for 30 minutes, add ethyl acetate dropwise to extract after the reaction is complete Three times, the extracts were combined and washed with saturated aqueous sodium chloride until neutral, dehydrated with anhydrous magnesium sulfate and...

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
sizeaaaaaaaaaa
Login to View More

Abstract

The invention relates to a method for separating chiral compounds by using molecular sieves, in particular to a separation method of calcitriol, alfacalcidol and esomeprazole sodium. Aiming at overcoming the defects of the existing separation technique, the invention provides a new method for separating the chiral compounds, which has the advantages of high yield and higher purity. By using different molecular sieves, chiral isomer impurities which are produced during preparation can be separated and removed. The method for separating chiral compounds by using molecular sieves has the advantages that the simple is simple and feasible, the pollution is small and the method is suitable for mass production.

Description

[technical field] [0001] The invention belongs to the technical field of drug synthesis and organic compound synthesis and preparation, and relates to a method for separating chiral compounds by using molecular sieves, in particular to a separation method for calcitriol, alfacalcidol and esomeprazole sodium. [Background technique] [0002] "Chirality", that is, chirality, is a term used to express the asymmetry of the configuration of a compound. It refers to the two forms in which the spatial arrangement of a compound molecule or certain groups in a molecule is in a mirror image relationship with its enantiomer but cannot overlap. Chiral drugs have good curative effect and few side effects. [0003] There are many separation methods of chiral enantiomers, such as chromatography, molecular imprinting, capillary electrophoresis, etc. Limitations, such as long time-consuming, large amount of solvent used, small amount of separation, etc. [0004] Calcitriol and alfacalcidol...

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 Applications(China)
IPC IPC(8): C07B57/00C07C401/00C07D401/12
Inventor 王明刚任莉陈阳生孙桂玉刘晓霞翟翠云
Owner CP PHARMA QINGDAO CO LTD
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