Crystal structure of 1-(benzyloxy)urea, C8H10N2O2

Xi Mai, Hong-Ying Xia, Yu-Sheng Cao, Xiao-San Lu, Yi-Jing Liao
2009 Zeitschrift für Kristallographie - New Crystal Structures  
C8H10N2O2, monoclinic, P12i/cl (no. 14), a = 12.456(3) Â, b = 5.008(1) Â, c = 13.681(4) k,ß = 96.017(4)°, V= 848.7 Â 3 , Z = 4, Rgt(F) = 0.057, wRreiF 2 ) = 0.166, T= 296 K. Source of material The title compound was synthesized by reaction of hydroxyurea (0.026 mol) with benzyl chloride (0.034 mol) in methanol (100 ml) in the presence of potassium hydroxide (0.034 mol). After refluxing for 13 h, the solution was distilled in the reduced pressure at 35 °C. The resulting crude solid was filtered
more » ... solid was filtered and washed by trichloromethane, then recrystallized in acetone/trichloromethane (5:2, v/v), filtered and dried. Colorless needle-shaped single crystals of the title compound suitable for X-ray structure determination were obtained by slow evaporation of the mixed solvent acetone/n-hexane (9:11, v/v) at room temperature for one week (m.p. 140 -142 °C). Experimental details H atoms were placed in calculated positions with d(C-H) = 0.93 (aromatic), 0.97 Â (methylene) and d(N-H) = 0.86 Â, and were refined in riding mode with i/iso(H) =1.2 U e q(C,N).
doi:10.1524/ncrs.2009.0238 fatcat:rhjokcgvr5brjji3qbo6lcdwci