Recently, considerable interest has been focused on the synthesis of new n-electron donors for the preparation of organic conductors.",'] In particular, tetrathiafulvalene (TTF) and its analogues have played a central role, and several TTF, tetraselena-, and dithiadiselena-fulvalene derivatives have been shown to have superconducting cation radical salts.12] We have recently synthesized bis-fused TTF, 2,5-bis ( (1) and furan (2) independently synthesized by three groups,'" are attractive extended TTFs because of the greatly reduced on-site Coulomb repulsion in the dicationic states and chalcogen-chalcogen interaction between 1,3-dithioles and central heteroaromatic rings. In this communication we report the synthesis and properties of several derivatives of bis-fused donors composed of TTF and 1 or 2 ( 3 a x and 4a-c).Synthesis of new donors 3a-c and 4a-c was achieved as shown in Scheme 1. Treatment of 5 with lithium diisopropylamide (LDA) in the presence of the aldehydes 6 and 719] afforded derivatives of 1 and 2 fused with 1,3-dithiol-2-one (8b,c and 9b,c) in 35-60% yields. The trimethylphosphite-mediated cross-coupling reactions between 8, 9 and 4,5-bis(methoxycarbonyl)-or 4,5-bis(methylthio)-1,3-dithiole-2-thiones (10b,c) in refluxing toluene gave the corresponding derivatives of 3 and 4 in 4 0 4 9 % yields."" The demethoxycarbonylation of tetrakis(methoxycarbonyl) derivatives 3b and 4b with an excess of LiBr-H 2 0 in HMPA at 90°C and then at 130°C afforded the parent derivatives 3a and 4a in 79 % and 60 % yields, respectively."'] All of these donors are stable in the solid