An improved, large-scale (90 g) synthesis of bis(tetraethylammonium)bis(1,3-dithiole-2-thione-4,5-dithiol)zincate: Synthesis and X-ray crystal structures of bicyclic and tricyclic 1,4-dithiocines derived from 1,3-dithiole-2-thione-4,5-dithiolate (DMI

摘要

An improved synthesis of bis(tetraethylammonium)bis(1,3-dithiole-2-thione-4,5-dithiol)zincate salt 2 is reported, and a new mechanism for the formation of 1,3-dithiole-2-thione-4,5-dithiolate (DMIT) disodium salt (1) is postulated. Three novel 1,4-dithiocine derivatives, 9, 11, and 13, were obtained by reaction of the zincate salt 2 with 1,4-dibromobutane-2,3-dione and 5,6-bis(bromomethyl)pyrazine-2,3-dicarbonitrile, and reaction of DMIT disodium salt 1 with 1,2-dibromo-4,5 -bis(bromomethyl)benzene: the single crystal X-ray structures of these 1,4-dithiocines are reported. [References: 19]