As eries of 7-diethylaminocoumarina mide compounds with phenyl (1), benzyl (2), and benzothiazole (3) terminal groups have been synthesized. The crystal structures of compounds 1 and 2 were determined by using single-crystalX -ray diffraction. All of these compounds exhibited intense blue fluorescence and high fluorescence quantum yields in both THF (1:0 .36, 2:0 .43, 3:0 .27) and high-viscositys olvent (glycerol; 1:0 .32, 2:0 .38, 3:0 .41). Compound 1 displayed bright-yellow-greenf luorescence, with af luorescencem aximum at l = 537 nm and aq uantum yield of 0.47 in the solid (powder) state. For compound 1, we observedared shift of Dl = 72 nm and fluorescence enhancement in the solid state relative to that in THF.C ompound 2 emitted bright-blue fluorescence( l = 463 nm, F = 0.36) in the solid state, which was slightly blue-shifted relative to that in THF (l = 466 nm vs l = 482 nm) and appeared as an arrow peak with af ull-width-at-half-maximum of only 39 nm. The strong fluorescencee mission in high-viscosity glycerols olution and in the solid state may be attributed to restriction of the rotation of the 7-diethylamino group, which led to non-radiativedeactivation.