Publisher Summary The synthetic compounds have large enough peripheral side chains to allow the formation of hydrophobic domains, which are believed to be important for the growth of directional chiral structures as e.g. also occurs in natural proteins. It appeared that by means of ultrafast time-resolved fluorescence spectroscopy, information could be obtained concerning the dynamics of excited-state intramolecular double proton transfer, the dynamics of excited-state solvation, and the influence of stacking on the chromophore fluorescent-state lifetime. This chapter extends time resolved fluorescence experiments to molecules TAB and DAC, in polar and apolar solvents. It is known that in polar chloroform, TAB remains in the molecularly dissolved state, but that in n-alkanes self-assembled chiral organized structures are formed. The experiments include the measurement of fluorescence transients under magic angle and polarization conditions. The data provide information concerning the excited-state intramolecular proton transfer dynamics in TAB and DAC, the lengthening of the lifetime of the fluorescent state by an order of magnitude upon chiral aggregation of the disk-shaped molecules TAB and DAC, and the dynamics of vibronic relaxation of TAB and DAC in the excited fluorescent state.