Synthesis and Crystal Structure of 4-(4-N N,-dimethyl)phenyl-7,7-dimethyl-5-oxo-3,4,5,6,7,8-hexahydrocoumorinone
Yuan Gao, Tu Shu
Abstract
Yuan Gao, Tu Shu
Abstract
The title compound (C19H23NO3) has been synthesized by the reaction of 4-N,N-dimethyl benzaldehyde, 5,5-dimethyl-1,3-cyclohexadione and meldrums in ethendiole for at 80℃ 2.5 hrs. Its structure was determined by single-crystal X-ray diffraction. The crystal is monoclinic, space group P21 with a=9.364(2), b=5.974(1), c=15.731(3)?, b=102.87(3)°, V=857.9(3) ?3, Z=2, Dc=1.213Mg/m3 , μ(MoKa)=0.082mm-1 , F(000)=336. The structure was solved by direct methods, and refined by full-matrix least-squares method to the final R=0.0521, wR=0.1392. X-ray analysis reveals that the dihedral angle between plane 1 (C(10)~C(15)) and plane 2 (C(5)-C6)-C(8)-C(9)-O(2)) is 88.77°, between plane 1 and plane 3 (C(1)-C(2)-C(4)-C(5)-C(9)) is 86.58° , between plane 2 and plane 3 is 1.86°.
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The title compound (C19H23NO3) has been synthesized by the reaction of 4-N,N-dimethyl benzaldehyde, 5,5-dimethyl-1,3-cyclohexadione and meldrums in ethendiole for at 80℃ 2.5 hrs. Its structure was determined by single-crystal X-ray diffraction. The crystal is monoclinic, space group P21 with a=9.364(2), b=5.974(1), c=15.731(3)?, b=102.87(3)°, V=857.9(3) ?3, Z=2, Dc=1.213Mg/m3 , μ(MoKa)=0.082mm-1 , F(000)=336. The structure was solved by direct methods, and refined by full-matrix least-squares method to the final R=0.0521, wR=0.1392. X-ray analysis reveals that the dihedral angle between plane 1 (C(10)~C(15)) and plane 2 (C(5)-C6)-C(8)-C(9)-O(2)) is 88.77°, between plane 1 and plane 3 (C(1)-C(2)-C(4)-C(5)-C(9)) is 86.58° , between plane 2 and plane 3 is 1.86°.
Key concepts: Chemistry, Monoclinic crystal system, Dihedral angle, Crystallography, Crystal structure, Crystal (programming language), Benzaldehyde, Plane (geometry)