Abstract In order to expand the repertoire of DNA sequences specifically interacting with transition metals, we report here the first examples of DNA sequences carrying mono‐ and bidentate phosphane ligands as well as P,N‐ligands. Aminoalkyl‐modified oligonucleotides have been reacted at predetermined internal sites with carboxylate derivatives of pyrphos, BINAP and phosphinooxazoline (PHOX) 2 b – d . Carbodiimide coupling in the presence of N ‐hydroxysuccinimide provided the DNA–ligand conjugates in 38–78 % yield. Phosphane‐containing oligonucleotides and their phosphane sulfide analogues were characterized by mass spectrometry (MALDI‐TOF and FT‐ICR‐ESI) and their stability after purification and isolation was systematically investigated. While DNA‐appended pyrphos ligand was quickly oxidized, BINAP and PHOX conjugates showed high stabilities, making them useful precursors for incorporation of transition metals into DNA.
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