The cyclization of 2-bromo-1-(1-naphthyl)undec-1-en-4,10-diyn-3-ol (I) by means of Pd(PPh3)4, CuI and Et2NH in hot acetonitrile gives the cyclodecadiyne derivative (II), which is acylated with acetic anhydride and DMAP in dichloromethane to yield the target acetate ester. Alternatively, the intermediate cyclodecadiyne derivative (II) can also be obtained by cyclization of 10-iodo-2-(1-naphthylmethylene)deca-3,9-diyn-1-al (III) by means of CrCl2 and NiCl2 in THF.