The intermolecular reductive coupling reaction of arylidenecyanoacetates induced by the TiCl4/Sm system was studied and the configuration of a cyclodimerisation product was confirmed by X-ray analysis.
ZhouL.H., ShiD. Q., GaoY., ShenW. B., DaiG. Y, and ChenW. X., Tetrahedron Lett.1997, 38: 2729
7.
GirardP., NamyJ. L., and KaganH. B., J. Am. Chem. Soc.1980, 102: 2693.
8.
Crystal data for 2d: C24H22Cl2N2O4, M = 473.35, colourless prismatic crystals, 0.2×0.2×0.3mm, Monoclinic, space group P21/c, a = 6.923(1), b = 33.178(5), c = 10.644(3)Å, β = 99.86(2)°, V = 2408.8(8) Å3, Z = 4, Dc = 1.305Mg/m3, μ = 3.01cm−1, F(000) = 984.00. Intensity data were collected on Rigaku AFC7R diffractometer with graohite-monochromated Mokα radiation (λ = 0.71069Å) using ω −2θ scan mode with 2θ max = 49.8°. 3308 unique reflections were measured and 2147 reflection with I >3σ (I) were used in the refinement. Refinement of positions and anisotropic thermal parameters for all non-hydrogen atoms (290 variables) converged to R = 0.052 and ωR = 0.067.
