Abstract
A practical one step procedure for the synthesis of 1,4-dioxane-2-one and 1,4-benzodioxine-2-one
derivatives is described.
Key words
alcohols - alkynes - diols - catalysis - cyclization
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X-ray crystal structure data for 11: Empirical formula: C15H10O3; Formula weight: 238.2; T = 293 (2) K, λ = 0.71073 Å; Crystal system = orthorhombic;
Space group: Pbca; Unit cell dimensions: a = 24.607 (8) Å, b = 12.508 (5) Å, c = 7.391 (4) Å, α = β = γ = 90.00°; V = 2274.8 Å3; Z = 8; Dcalc = 1.391g/cm3; Absorption coefficient: 0.097 mm-1; F(000) = 992; Crystal size: 0.65 × 0.45 × 0.15 mm; Reflections collected: 14778;
Independent reflections: 2528 [R(int) = 0.0194]; Refinement method, full-matrix least-squares on F2; Goodness-of-fit
on F2: 1.034; Final R indices [I > 2σ(I)] R1 = 0.0420, wR2 = 0.1005; R indices (all data) R1 = 0.0659, wR2 = 0.1157; Extinction coefficient: 0.021 (2); Largest diff. peak and hole: 0.144
and -0.145e Å-3.