A series of oligoethylene glycols, incorporating two pendant naphthyl groups along the interior of the chain using a phosphate triester linkage, have been prepared. The synthetic methodology has been discussed in the context of eventually providing a route to polymers labeled in a similar fashion. The steady state fluorescence behavior of these compounds is reported briefly. Relatively little excimer emission is observed. The synthetic intermediates to the phosphates, the 2-(1-naphthyl)ethyl N,N-diisopropylphosphoramidites of triethylene glycol and tetraethylene glycol, show exciplex fluorescence. The fluorescence from these latter compounds exhibits some sensitivity to solvent quality.