Synthesis of 2,4-Disubstituted Thiophenols and Solid State Structures of Thiocarbamate Precursors

A series of thiophenols with different ortho-substituents, 2,4-dimethylthiophenol, 2-tert-butyl-4-methylthiophenol, and 2-(1-adamantyl)-4-methylthiophenol, which display varying degrees ofsteric hindrance on the 2-position, was prepared from the corresponding phenols. Initial deprotonationof the phe...

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Detalles Bibliográficos
Autores: Aarón Flores Figueroa, Víctor Arista-M, Daniel Talancón Sánchez, Ivan Castillo
Tipo de recurso: artículo
Estado:Versión publicada
Fecha de publicación:2005
País:México
Institución:Universidad Nacional Autónoma de México
Repositorio:Redalyc-UNAM
OAI Identifier:oai:redalyc.org:47549213
Acceso en línea:https://www.redalyc.org/articulo.oa?id=47549213
Access Level:acceso abierto
Palabra clave:Química
thiols
thiophenols
bulky thiols
ray structure
thiocarbamates
Descripción
Sumario:A series of thiophenols with different ortho-substituents, 2,4-dimethylthiophenol, 2-tert-butyl-4-methylthiophenol, and 2-(1-adamantyl)-4-methylthiophenol, which display varying degrees ofsteric hindrance on the 2-position, was prepared from the corresponding phenols. Initial deprotonationof the phenols was achieved with NaH in dimethoxyethane, followed by treatment with N,Ndimethylthiocarbamoylchloride, to obtain the O-arylthiocarbamates. Thermolysis of the lattercompounds resulted in rearrangement, which yields the desired S-arylthiocarbamates. Finally,reduction of the S-arylthiocarbamates with LiAlH4 in THF, followed by acidic workup, allowed theisolation of the thiophenols. All products were characterized by spectroscopic techniques, and in thecase of some of the thiocarbamates the solid state structures were determined by single-crystal X-raydiffraction.