1 13 H and C NMR spectra of six dialkylaminoarsolanes were obtained as a function of solvent, concentration, and temperature. CI mass spectral data were also obtained as a function of retention time for the same compounds. These results suggest that the AsN bond is not labile as compared to the AsCl bond in chloroarsolanes. No evidence for dimer formation was noted either in solution or the gas phase under the investigated experimental conditions. The averaged solution conformation of the 1,3-dioxarsolane ring is discussed in terms of rapid intramolecular conformational averaging; nature of substituents at the 2,4, and 5 positions; and effects of temperature, solute concentration and solvent type. © 1985.