0000000000496481
AUTHOR
Pascale Tavares
ChemInform Abstract: Synthesis of the First Benzodiselenagermoles and One Spirobisdiselenagermole.
Abstract The first examples of compounds R1R2GeSe2C6H4R3 (R1,R2=CH3 C2H5, C3H2, n-C4H9, i-C5H11, Ph, p-CH3Ph. R3=H, CH3, OCH3) were easily obtained (40–80% yield) from electrophilic cleavage of diselenophenylene zirconocenes by dialkyl or diaryl dichlorogermanes. The synthesis of a spirodi-selenagermole was achieved in the same way using germanium tetrachloride. Analytical data, 1H and 77Se NMR. mass spectra are perfectly consistent with the expected structures.
Synthesis ofo-thiatelluraphenylenezirconocenes. X-ray crystal structure of
o-Thiatelluraphenylenezirconocene complexes were obtained in good yield by reaction of dilithiumo-benzenthiatelluride with zirconocene dichlorides. These compounds represent the first examples of heterodichalcogenaphenylene bent metallocences. They were characterized by spectroscopic methods and the effect on the n.m.r. results of stepwise substitution of one and two Te atoms for S is discussed.
Benzodiselenagermoles and spirobisbenzodiselenagermoles
Synthesis of benzodiselenagermoles and bisbenzodiselenagermoles was carried out by transmetallation group 4 group 14 between diselenophenylenezirconocenes and dialkyl-, diaryl- or alkylaryldichlorogermanes, aryltrichlorogermane or germanium tetrachloride. The new compounds were studied by 1H, 77Se NMR and mass spectrometry. In the case of compounds with substituted phenyl groups, double irradiation and 2D NMR experiments were performed to determine the chemical shifts of the two selenium atoms. The crystal structure of a spirobisbenzodiselenagermole has been established by X-ray diffraction analysis.