A series of diphenylamino-substituted phenylene-(poly) ethynylenes were successfully synthesized by a combination of Sonogashira coupling and double elimination protocol of β- substituted sulfones. When UV-light was irradiated, the amino-substituted phenylene-(poly) ethynylene emitted strong luminescence. The emission underwent a large bathochromic shift in polar solvent because of stabilization of their charge-separated excited states. ...