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

Purification method of 2-deoxidation-L-ribose

A purification method and ribose technology, applied in the direction of deoxy/unsaturated sugar, chemical instruments and methods, sugar derivatives, etc., can solve the problem of low purity of 2-deoxy-L-ribose, absence of 2-deoxy-L-ribose, There are many side reactions, etc., to achieve the effect of improving product purity, less control process, and simple operation

Active Publication Date: 2013-12-11
济南尚博医药股份有限公司
View PDF9 Cites 2 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

2-Deoxy-L-ribose is an important intermediate in the synthesis of new biologically active L-nucleoside drugs, which can be used in the study of protein-DNA interaction, and in important anti-sensitive drugs such as enantiomer DNA (enantio- DNA) or meso-DNA (meso-DNA) is used as a basic building block, and nucleoside derivatives formed with organic bases such as adenine have great application potential in the treatment of cancer and hepatitis B. However, 2 - Deoxy-L-ribose does not exist in nature and can only be obtained through synthetic methods
However, since 2-deoxy-L-ribose has many side reactions during the synthesis process, the purity of 2-deoxy-L-ribose is low

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
  • Purification method of 2-deoxidation-L-ribose
  • Purification method of 2-deoxidation-L-ribose
  • Purification method of 2-deoxidation-L-ribose

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] 1) Dissolve 100 g of the crude product 2-deoxy-L-ribose in 400 g of deionized water, and stir until dissolved;

[0031] 2) Add 600g of methanol and stir for 15min. Add 150 g of aniline and stir for 5 h at 20-25°C. Cool down and crystallize, stir at 0-5°C for 5h;

[0032] 3) filter, and wash the filter cake twice with deionized water, each time with 80 g of deionized water;

[0033] 4) Add the filter cake to 1000g of water and stir until uniform. Add 350g of strong acid resin, stir until dissolved at 20-25°C;

[0034] 5) filter, and wash the filter cake twice with deionized water, each time with 50 g of deionized water;

[0035] 6) The filtrate was extracted three times with dichloromethane, each time using 200 g, and the phases were separated. The aqueous phase was neutralized to pH=6.5 with saturated sodium bicarbonate solution;

[0036] 7) Distilled water under reduced pressure, until the syrup quality is 250g, stop distilling water;

[0037] 8) Cool down to 20...

Embodiment 2

[0046] 1) Dissolve 100 g of the crude product 2-deoxy-L-ribose in 600 g of deionized water, and stir until dissolved;

[0047] 2) Add 540g of methanol and stir for 15min. Add 120 g of aniline and stir for 5 h at 20-25°C. Cool down and crystallize, stir at 0-5°C for 5 hours;

[0048] 3) filter, and wash the filter cake twice with deionized water, each time with 100 g of deionized water;

[0049] 4) Add the filter cake to 1200g of water and stir until uniform. Add 300g of strong acid resin, stir until dissolved at 20-25°C;

[0050] 5) filter, and wash the filter cake twice with deionized water, each time with 40 g of deionized water;

[0051] 6) The filtrate was extracted three times with ethyl acetate, each time using 150 g, and the phases were separated. The aqueous phase was neutralized to pH=7 with saturated sodium bicarbonate solution;

[0052] 7) Distilled water under reduced pressure, until the syrup quality is 300g, stop distilling water;

[0053] 8) Cool down to ...

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

No PUM Login to View More

Abstract

The invention discloses a purification method of 2-deoxidation-L-ribose, which comprises the steps of dissolving a crude product, namely 2-deoxidation-L-ribose in deionized water, adding methanol and aniline, reacting to form salt, filtering, washing, adding the deionized water and highly-acid resin, stirring till dissolution, filtering, washing, extracting a solvent from a filtrate, separating a phase, removing aniline in a solution, neutralizing, decompressing, concentrating, cooling, adding tert-butyl methyl ether, cooling, crystallizing, leaching, washing the solvent, performing vacuum drying at a low temperature, and obtaining purified 2-deoxidation-L-ribose. The method is simple to operate, few in intermediate control process and high in safety, and the product purity is improved greatly and can achieve above 98%.

Description

technical field [0001] The invention relates to the technical field of organic synthesis, in particular to a method for purifying 2-deoxy-L-ribose. Background technique [0002] 2-Deoxy-L-ribose is an important intermediate in chemical and pharmaceutical industries, and its derivatives are used in medical, food and other industries. 2-Deoxy-L-ribose is an important intermediate in the synthesis of new biologically active L-nucleoside drugs, which can be used in the study of protein-DNA interaction, and in important anti-sensitive drugs such as enantiomer DNA (enantio- DNA) or meso-DNA (meso-DNA) is used as a basic building block, and nucleoside derivatives formed with organic bases such as adenine have great application potential in the treatment of cancer and hepatitis B. However, 2 -Deoxy-L-ribose does not exist in nature and can only be obtained through synthetic methods. However, since 2-deoxy-L-ribose has many side reactions during the synthesis process, the purity of...

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): C07H3/08C07H1/06
Inventor 孟庆文顾振磊郗遵波
Owner 济南尚博医药股份有限公司
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