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Oligonucleotides containing (2′‐deoxy‐β‐D‐xylofuranosyl)guanine have been prepared. For this purpose 2‐aminoadenosine (5) was synthesized and converted to 2′‐deoxy‐β‐D‐xyloguanosine (1). The related 2′‐deoxy‐β‐D‐xyloisoguanosine (3) and 2′‐deoxy‐β‐D‐xyloxanthosine (4) were also synthesized. Compound 1 was converted to the phosphonate and phosphoramidite building blocks 10 and 11, respectively. The oligodeoxynucleotide (5′‐3′)d(xG‐xT‐xA‐xG‐xA‐xA‐xT‐xT‐xC‐xT‐xA‐xC‐T) (18) formed a duplex with the same Tm as the parent (5′‐3′)‐(G‐T‐A‐G‐A‐A‐T‐T‐C‐T‐A‐C) (19), but with an inverted CD spectrum.

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A monomeric dialuminoxane with a linear AlOAl group and a planer C2AlOAlC2 framework is a description of the title compound 1. Four bulky substituents provide strong steric protection. Dialuminoxane 1 arises by insertion of an oxygen atom into the AlAl bond of the corresponding dialuminum derivative. Crystal structure data and NMR spectra suggest a π interaction between aluminum and oxygen.