目的：建立了在水相中,通过微波辅助的多组分反应一步合成吡啶酮衍生物的方法;方法：以芳醛、1,3-二羰化合物、麦氏酸和醋酸氨为起始原料,在水相中,通过微波辅助的多组分反应一步合成吡啶酮及其衍生物.结果：反应在3-8 m in内完成,产率优良81-95%,产物结构经红外,核磁和元素分析得以确证.结论：该方法具有反应时间短,产率高,操作简单,环境友好等优点.
The title compounds have been synthesized via a three-component reaction and their structures were characterized by IR,1H NMR,13C NMR and X-ray single-crystal diffraction. The crystal of compound 4a belongs to monoclinic,space group P121/c1 with a = 8.575(3),b = 9.590(3),c = 21.431(6) ,β = 91.172(3)°,V = 1762.1(9) 3,Mr = 393.36,Z = 4,Dc = 1.483 g/cm3,μ(MoKα) = 0.113 mm-1,F(000) = 816,the final R = 0.0366 and wR = 0.0941. The crystal of compound 4b is of triclinic,space group P-1 with a = 8.6420(17),b = 9.761(2),c = 11.132(2),α = 97.51(3),β = 97.86(3),γ = 92.85(3)°,V = 920.1(3) 3,Mr = 393.36,Z = 2,Dc = 1.420 g/cm3,μ(MoKα) = 0.108 mm-1,F(000) = 408,the final R = 0.0612 and wR = 0.1781. In each molecular structure,the naphthalene rings and pyran rings are almost coplanar with the latter in an envelope conformation. The rings formed by the N-H···O intramolecular hydrogen bonds are almost planar in these compounds. Their crystal packing is stabilized by intermolecular hydrogen bonds together with C-H···π and π-π stacking interactions.
The solvents for the separation of diphenyl and 4-phenylacetophenone were screened with computer according to the solid-liquid equilibrium equation based on UNIFAC.With the predicted separation factor values and selection principle for feasible solvents,the candidates of better solvents were determined as n-heptane,n-hexane,cyclohexane and diisopropyl ether.The solubility and separation factor of the two solid solutes in n-heptane,n-hexane,cyclohexane,diisopropyl ether and ethanol were measured by static equilibrium method.The average relative deviation between the calculated separation factor and experimental data is 16.73%,indicating that the solid-liquid equilibrium equation based on UNIFAC is suitable to select the separation solvent for solid solute mixtures with similar molecule stereoscopic structures.
The title compound 5-cyclopropyl-10-(4-fluorophenyl)-7,7-dimethyl-7,8-dihydro- 5H-indeno[1,2-b]quinolne-9,11(6H,10H)-dione was obtained by the reaction of 4-fluorobenzal- dehyde, 2H-indene-1,3-dione and 3-(cyclopropylamino)-5,5-dimethylcyclohex-2-enone in the presence of acetic acid under microwave irradiation. Its structure was confirmed by IR and 1H- NMR spectra. The crystal is of monoclinic, space group P21/c with a = 14.138(3), b = 8.952(2), c = 17.140(3) , β = 102.253(3)o, C27H24FNO2, Mr = 413.47, Z = 4, V = 2119.9(8) 3, Dc = 1.296 g/cm3, μ(MoKα) = 0.087 mm-1, F(000) = 872, the final R = 0.0425 and wR = 0.0905 for 2336 observed reflections (I > 2σ(I)). X-ray analysis revealed that the pyridine ring adopts a boat conformation and the six-membered ring fused with it assumes a twist boat conformation.
