Aliphatic Sulphonic Acid Salt Catalyst for Nucleoside Synthesis

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Solution Overview

Problem

Existing methods for synthesizing nucleosides using catalysts like SnCl4, TiCl4, and trialkylsilyl esters face issues with hydrolysis, irritant byproducts, and handling difficulties, especially in large-scale production, due to the formation of insoluble oxides and reactive silylating agents.

Innovation Solution

The use of a salt of an aliphatic sulphonic acid, such as lithium trifluoromethanesulfonate, as a catalyst for reacting a silylated nucleoside base with a glycoside donor, which is stable under aqueous conditions, easy to handle, and does not produce irritant hydrolysis products, allowing for high selectivity and yield in nucleoside production.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Reliability

If traditional catalysts like SnCl4, TiCl4, or trialkylsilyl esters are used for nucleoside synthesis, then the reaction can proceed, but the catalysts are prone to hydrolysis producing irritant byproducts and insoluble oxides that are difficult to remove

Engineering Contradiction:
Improvecatalyst stabilityVSAvoidhydrolysis byproducts
Core Design Contradiction:
ReliabilityVSObject-generated harmful factors

Solution Approach 1:

The patent changes the chemical nature of the catalyst from traditional Lewis acids (SnCl4, TiCl4) or silyl esters to aliphatic sulphonic acid salts. This parameter change in catalyst type fundamentally alters the reaction system, eliminating hydrolysis susceptibility while maintaining catalytic activity for glycoside bond formation.

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The aliphatic sulphonic acid salts used as catalysts are water-soluble and can be easily removed from the reaction mixture through simple filtration or extraction, eliminating the need for complex purification steps to remove insoluble oxide byproducts. The catalyst itself remains stable and reusable.

Inventive Principle:
Principle #27Cheap short-living objects (Disposable)

2Power

If trialkylsilyl esters are used as catalysts, then the reaction can be catalyzed, but the silylating agents are very reactive and quickly react to form the ester, complicating handling and purification

Engineering Contradiction:
Improvecatalytic activityVSAvoidhandling difficulty
Core Design Contradiction:
PowerVSEase of operation

Solution Approach 1:

The aliphatic sulphonic acid salts serve as stable, non-reactive catalysts that do not undergo rapid side reactions. Their water solubility allows for easy handling and simple removal from the reaction mixture through filtration or extraction, eliminating the handling difficulties associated with reactive silylating agents.

Inventive Principle:
Principle #27Cheap short-living objects (Disposable)

3Productivity

If traditional catalysts are used for large-scale production, then nucleosides can be synthesized, but the catalysts are difficult to handle and remove, increasing process complexity

Engineering Contradiction:
Improveproduction rateVSAvoidprocess complexity
Core Design Contradiction:
ProductivityVSDevice complexity

Solution Approach 1:

The patent changes the catalyst properties to be water-soluble and non-hydrolyzing, which fundamentally simplifies the work-up process. The catalyst can be easily removed from the reaction mixture through simple filtration or extraction, eliminating complex purification steps and reducing overall process complexity for large-scale production.

Inventive Principle:
Principle #35Parameter changes

Applied Scientific Principles

This section explains which scientific principles are used to turn an abstract innovation direction into a practical engineering solution.

Function Achieved in This Case

This approach results in a reaction yield higher than 95% with excellent alpha/beta anomer selectivity and simplifies the production process by eliminating the need for ester compounds, making it suitable for large-scale production without the challenges of handling reactive catalysts.

Implementation Method 1

reacting a protected, preferably silylated, nucleoside base with a glycoside donor, preferably a 1-halogen derivative, or 1-0-acyl, 1-0-alkyl, or an imidate preferably a trichloromethyl imidate, or a thio-alkyl derivative of a blocked monosaccharide or oligosaccharide, preferably ribose and 2-desoxyribose derivatives, in the presence of a selected catalyst

Methodology Applied
Scientific EffectCatalysis: Catalysis

Data Source

PatentEP2197892B1Method of producing nucleosides
Publication Date: 2014.07.16 CILAG AG

AI summary

Method of producing a free nucleoside compound, the compound 2'- deoxy-5-azacytidine (Decitabine) being excluded, by reacting a glycoside donor preferably a 1-halogen derivative, or 1-0-acyl, 1-0-alkyl, or an imidate preferably a trichloromethyl derivative, or a thio-alkyl derivative of a blocked monosaccharide or oligosaccharide preferably ribose and 2-desoxyribose derivatives with a protected nucleoside base, in a suitable anhydrous solvent and in the presence of a catalyst, and removing the protecting groups from said blocked nucleoside compound, wherein said catalyst is selected from the group comprising salts of an aliphatic sulphonic acid and/or salts a strong inorganic acid containing a non-nucleophilic anion.