Lh. Yu et Db. Zhu, FURTHER INVESTIGATIONS ON THE SYNTHESIS AND CHARACTERIZATION OF VINYLOGUES OF BIS (ETHYLENEDITHIO) TETRATHIAFULVALENE, Phosphorus, sulfur and silicon and the related elements, 116, 1996, pp. 225-234
A strong electron pi-donor, vinylogue bis (ethylenedithio) tetrarhiafu
lvalene (4) has been obtained in a six-step from 4,5-bis(benzoylthio)
1,3-dithiole-2-thione (7) (ca. 40% overall yield), its structure was f
ully characterized by (1)HNMR, FT-IR, MS(EI) and elemental analysis. T
he yield for the starting material TEA(2)[Zn(DMIT)(2)](2) is enhanced
to 95% by an improved synthetic procedure described herein. Synthesis
of aldehyde 14 was investigated in different solvent systems. Compound
10 and the new Horner-Wittig phosphonate (13) were first purified as
a solid.