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The palladium‐mediated coupling of p‐ethynylphenylalanine (p‐epa) with different halogenated benzenes yielded alkyne‐bridged α‐amino acids. A series of cationic mono‐ to hexanuclear (Ph3P)2Pt complexes with the anions of p‐ethynylphenylalanine and alkynyl‐ or benzene‐bridged di‐, tri‐, tetra‐ and hexa‐ethynyl phenylalanines as N,O‐chelate ligands was prepared. N‐t‐Boc‐p‐ethynylphenylalanine methyl ester was metal‐substituted to give complexes of the types Ph3PAu‐C≡C–R and (Et3P)2Pt(C≡CR)2. The benzene‐bridged di‐, tri‐, tetra‐ and hexa‐p‐ethynylphenylalanine methyl esters form Schiff bases with ferrocene aldehyde and a tripodal ligand was obtained from Ph2PCH2CH2CH2NH2 and the benzene‐bridged tri‐ethynylphenylalanine. The structure of (Ph3P)2Pt[NH2C(H)(CH2C6H4C≡CH)CO2]+ BF4− was determined by X‐ray diffraction.

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