A new compound, 2-dichloromethyl-2-p-nitrophenyl-1,3-dioxane, was synthesized and characterized. The crystal structure of the title compound (C11H11Cl2NO4,Mr=292.11) has been determined by single-crystal X-ray diffraction. The crystal is of monoclinic, space groupP21/cwitha=11.013(2) Å,b=14.653(3) Å,c=7.8693(16) Å,α=90°,β=97.06(3)°,γ=90°,V=1260.3(4) Å3,Z=4,F(000)=600,Dc=1.540 mg/cm3, the finalR1=0.0508, andωR2=0.1072for observed reflections withI>2σI. A total of 12162 reflections were collected, of which 2867 were unique (Rint=0.06999).