A series of α, ω-diphenylpolyynes were synthesized through the Cadiot Chodkiewicz reaction starting from Cu(I)-phenylacetylide and diiodoacetylene. The complete series of diphenylpolyynes Phi-(CC)n-Phi with n = 2,3,4 and 5 was obtained and analyzed by electronic absorption spectroscopy, liquid chromatography (HPLC-diode array) and FT-IR spectroscopy. The diphenylpolyynes when treated with nascent hydrogen produced by the action of HCl on Zn dust are changed into a mixture of diphenylpolyenes as shown by UV spectroscopy and HPLC
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