4-(4-N,N-二甲胺基)苯基-7,7-二甲基-5-氧代-3,4,5,6,7,8-六氢香豆素酮的合成和晶体结构

标题化合物C19H23NO3由4-N,N-二甲胺基苯甲醛、5,5-二甲基-1,3-环己二酮、麦氏酸在乙二醇中于80℃反应2.5小时而得。结构通过单晶X-射线衍射法确定,其晶体属单斜晶系, C19H23NO3，空间群P21, 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。晶体结构用直接法解出，经用全矩阵最小二乘法对原子参数进行修正，最终的偏离因子为R=0.0521, wR=0.1392。在分子结构中，存在3个平面, C(10)~C(15)构成平面1，C(5)-C6)-C(8)-C(9)-O(2)构成平面2，C(1)-C(2)- C(4)-C(5)-C(9)构成平面3，平面1与平面2的最小二乘面的两面角为88.77°，平面1与平面3的最小二乘面的两面角为86.58°，平面2与平面3的最小二乘面的两面角为1.86°.

Synthesis and Crystal Structure of 4-(4-N N,-dimethyl)phenyl-7,7-dimethyl-5-oxo-3,4,5,6,7,8-hexahydrocoumorinone

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°.