Sulfonium Salt Synthesis for Fluorinated Drug Precursors

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Solution Overview

Problem

Current methods for preparing sulfonium salts are limited by their reactivity with basic functional groups, making it difficult to functionalize organic compounds containing complex functionalities, and the introduction of fluorine or radioactive fluorine-18 into aromatic compounds is challenging due to low yields, poor selectivity, and high costs.

Innovation Solution

A method involving the formation of sulfonium salts with a dibenzothiophene ring and basic groups, allowing for the introduction of nucleophiles under mild conditions, and the use of sulfonium salts as precursors for fluorination, including the use of fluoride-18, without the need for protecting groups, facilitating the synthesis of complex functionalized compounds.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Ease of manufacture

If conventional methods (Grignard reactions, acid-catalysed reactions) are used to prepare sulfonium salts, then simple sulfonium salts can be obtained, but the methods are not compatible with molecules containing basic functional groups due to high reactivity of reagents

Engineering Contradiction:
Improvepreparation of sulfonium saltsVSAvoidcompatibility with functional groups
Core Design Contradiction:
Ease of manufactureVSAdaptability or versatility

Solution Approach 1:

The patent changes the chemical parameters of the reaction system by using electrophilic aromatic substitution with aryl halides and palladium catalysts instead of highly reactive Grignard reagents or strong acids. This parameter change allows the reaction to proceed under milder conditions that are compatible with basic functional groups like amines, thereby resolving the contradiction between ease of manufacture and adaptability to different functional groups.

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The patent introduces a palladium catalyst as an intermediary to mediate the coupling reaction between aryl halides and sulfides. This catalyst enables the formation of sulfonium salts under milder conditions without requiring highly reactive reagents that would interfere with basic functional groups, thus allowing both easy preparation and broad functional group compatibility.

Inventive Principle:
Principle #24Intermediary (Mediator)

2Reliability

If protecting group methodology is used to prevent interference of reactive functional moieties, then sulfonium salts can be prepared, but the number of synthetic steps increases

Engineering Contradiction:
Improveprevention of functional group interferenceVSAvoidnumber of synthetic steps
Core Design Contradiction:
ReliabilityVSDevice complexity

Solution Approach 1:

The patent extracts the problem of functional group interference by developing a reaction system that is inherently tolerant of basic functional groups. Instead of adding protecting groups to remove the interference problem, the methodology directly addresses it by using mild electrophilic substitution conditions that do not react with or interfere with basic groups, thereby eliminating the need for additional protection and deprotection steps.

Inventive Principle:
Principle #2Taking out (Extraction)

Solution Approach 2:

Rather than protecting functional groups before sulfonium salt formation (conventional approach), the patent inverts the strategy by using reaction conditions that are specifically designed to be compatible with unprotected functional groups. This inversion eliminates the need for protecting group methodology and reduces the overall number of synthetic steps.

Inventive Principle:
Principle #13The other way round (Inversion)

3Quantity of substance

If conventional fluorination methods (diazonium salts, electrophilic agents, transition metal catalysts) are used, then fluorinated compounds can be obtained, but yields are low, selectivity is poor, or expensive reagents and harsh conditions are required

Engineering Contradiction:
Improveintroduction of fluorineVSAvoidyield and selectivity
Core Design Contradiction:
Quantity of substanceVSProductivity

Solution Approach 1:

The patent uses the sulfonium salt as a precursor that copies the desired fluorinated product structure, allowing for high-yield nucleophilic substitution with fluoride ions. This approach avoids the low yields and poor selectivity of conventional fluorination methods by using a pre-functionalized intermediate that is specifically designed for efficient fluoride displacement.

Inventive Principle:
Principle #26Copying

Solution Approach 2:

The patent performs preliminary action by first installing the sulfonium group as a leaving group before introducing fluorine. This two-step sequence (sulfonium salt formation followed by nucleophilic substitution) allows for better control and higher yields compared to direct fluorination methods, as the sulfonium group provides an excellent leaving group that facilitates clean substitution with fluoride ions.

Inventive Principle:
Principle #10Preliminary action

4Quantity of substance

If costly functionalised fragments are used at early stages to introduce fluorine, then fluorinated compounds can be prepared, but the cost of desired molecules increases

Engineering Contradiction:
Improveintroduction of fluorineVSAvoidcost of synthesis
Core Design Contradiction:
Quantity of substanceVSEase of manufacture

Solution Approach 1:

The patent performs preliminary action by installing the sulfonium precursor group early in the synthesis using inexpensive aryl halides and sulfides, then introduces fluorine in a later high-yield substitution step. This approach avoids the need to use costly fluorinated fragments at early stages, as the fluorine is introduced efficiently from inexpensive fluoride sources in a controlled nucleophilic substitution reaction.

Inventive Principle:
Principle #10Preliminary action

Solution Approach 2:

The patent uses the sulfonium salt as a temporary placeholder or 'copy' of the desired fluorinated product, allowing the molecule to be assembled with inexpensive precursors and then converted to the final fluorinated product in a high-yield step. This copying strategy avoids the accumulation of cost that would result from using expensive fluorinated building blocks throughout the synthesis.

Inventive Principle:
Principle #26Copying

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

Enables the preparation of sulfonium salts with unprotected basic functionalities and allows for facile reactions with nucleophiles, enabling the introduction of fluorine or radioactive fluorine-18 into complex organic compounds, reducing synthesis steps and costs while improving yields and selectivity.

Implementation Method 1

The sulfonium salts undergo facile reactions with nucleophiles, enabling the introduction of fluorine or radioactive fluorine-18 into complex organic compounds

Methodology Applied
Scientific EffectNucleophilic substitution: Chemical Bonding

Data Source

PatentEP2906548B1Compounds and their synthesis
Publication Date: 2019.12.04 UCL BUSINESS LTD
  • EP2906548B1 patent drawingFigure 1
  • EP2906548B1 patent drawingFigure 2
  • EP2906548B1 patent drawingFigure 3A~3B

AI summary

The present invention relates to sulfonium salts of formula (I): (I), their preparation, and utility as precursors for preparing functionalised organic compounds, wherein R1 and R2 are the same or different and each is independently selected from an optionally substituted aryl group, an optionally substituted alkynyl group, an optionally substituted alkenyl group, an optionally substituted alkyl group, an optionally substituted cycloalkyl group, an optionally substituted cycloalkenyl group, an optionally substituted aralkyl group, an optionally substituted arylalkenyl group, an optionally substituted heteroaryl group, an optionally substituted heterocyclyl group, an optionally substituted amine, an optionally substituted alkoxy group, an optionally substituted thioether group, an optionally substituted phosphine group, an optionally substituted boron species, an optionally substituted carbene, an organometallic moiety, and a halide, or R1 and R2 are joined together to form an optionally substituted sulfur-containing ring; W is a bond, an optionally substituted alkynylene group, an optionally substituted alkenylene group, and optionally substituted alkylene group, an optionally substituted heterocyclyl group, an optionally substituted aryl group or an optionally substituted heteroaryl group; R3 is a moiety comprising at least one basic group, provided that when R3 does not contain any carbon atoms, W is not a bond; X is an anionic species; and n is an integer selected from 1 to 5.