The title compound has been synthesized by alkylation of diphenylglycoluril with o-xylylenedihalides followed by Sonogashira cross-coupling reaction. The yielded product 2 was investigated with X-ray crystallographic, NMR, EI-MS, and IR techniques. The crystal belongs to a triclinic system, space group P-1 with unit cell parameters a = 10.5057(8) Å, b = 12.6915(9) Å, c = 13.3426(10) Å, α = 83.8540(10)o, β = 87.9360(10)o, γ = 75.5700(10)o, V = 1712.9(2) Å3, Z = 2, Dc = 1.322, Mr = 681.59, μ = 0.232 mm−1, F(000) = 708, R1 = 0.0586 and wR2 = 0.1470.Graphical Abstract:Two molecules of 2 undergo dimerazation due to the formation of two self-complementary N–H···O = C interactions to yield the R22(8) hydrogen bonding motif.