Synthesis method of tris (p-tolyl) sulfonium hexafluorophosphate

By employing Grignard reaction and recrystallization processes, the problem of low yield in the synthesis of tri(p-tolyl)thionium hexafluorophosphate was solved, achieving high-yield and high-purity product preparation suitable for large-scale production.

CN122079841APending Publication Date: 2026-05-26HEBEI UNIV OF SCI & TECH
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Patent Information

Application Number
CN202610495892.X
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2026-04-15
Publication Date
2026-05-26

AI Technical Summary

Technical Problem

Existing methods for synthesizing tri(p-tolyl)thionium hexafluorophosphate have low yields, high costs, and are difficult to produce on a large scale. They also produce a large number of mono- and di-substituted byproducts.

Method used

Tris(p-tolyl)thionium bromide was prepared by Grignard reaction of bis(4-chlorophenyl) sulfoxide and p-tolyl magnesium bromide in the presence of trimethylchlorosilane, and then by recrystallization with potassium hexafluorophosphate and ethyl acetate/n-hexane.

Benefits of technology

The yield of tri(p-tolyl)thionium hexafluorophosphate was increased to 71.34%. The raw materials are readily available, the activation conditions are mild, the production safety is high, the crystal form is improved, the oiling phenomenon is reduced, and the product purity is improved.

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Abstract

The invention discloses a synthesis method of tris (p-methylphenyl) sulfonium hexafluorophosphate, which comprises the following steps: uniformly mixing bis (4-chlorphenyl) sulfoxide and a solvent, slowly adding p-methylphenyl magnesium bromide in an inert atmosphere, stirring to react for 10 minutes, dropwise adding trimethylchlorosilane, dropwise adding a 25 wt% hydrobromic acid aqueous solution to quench after the reaction is completed, filtering, washing, and drying to obtain the tris (p-methylphenyl) sulfonium hexafluorophosphate. Carrying out extraction and vacuum concentration to obtain tri (p-tolyl) sulfonium bromide; adding a potassium hexafluorophosphate aqueous solution into the tri (p-tolyl) sulfonium bromine salt, carrying out a stirring reaction, carrying out suction filtration after the reaction is finished, and recrystallizing a filter cake to obtain tri (p-tolyl) sulfonium hexafluorophosphate; according to the method, the raw materials are cheap and easy to obtain, the activation condition is mild, the production safety is high, and the yield of the prepared tri (p-tolyl) sulfonium hexafluorophosphate can reach 71.34% at most.
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