A facile and practical method for the synthesis of ArC≡ CCF 3 is described which involves (1) conversion of aldehydes ArCHO into ArCH= CClCF 3 with 1, 1, 1-trichloro-2, 2, 2- trifluoroethane, zinc powder, and acetic anhydride in one-pot and (2) dehydrochlorination with sodium t-butoxide or sodium amide/t-butyl alcohol.