摘要
A novel method for the synthesis of novel silalactone was proposed by iodation and zirconium-mediated cycloaddition of alkynes. 1,1-Dimethyl-4-carboxylatethyl-6,7-diphenyl-5-(trimethylsilyl)-1,3-dihydrobenzo[c][1,2]oxasilol-3(1 H)-one(compound 1) was obtained and characterized by X-ray single-crystal diffraction. It belongs to the monoclinic system, space group P2_1/n with a = 12.706(3), b = 10.826(2), c = 19.407(4) A, β = 91.50(3)°, V = 2668.4(9) A^3, Z = 4, F(000) = 1004, D_c = 1.182 mg/m^3, μ = 0.162 mm^-1, T = 293(2) K, S = 1.129, R = 0.0868 and wR = 0.1607 for 3542 observed reflections with I 〉 2σ(I). The butadiene derivative, 3,6-di(2-methylphenyl)-4,5-diethylocta-3,5-diene(compound 2), was synthesized by zirconacyclopentadiene and aryl iodides in the presence of Cu Cl and Pd(PPh3)4. It was characterized by X-ray single-crystal diffraction for the first time, belonging to the monoclinic system, space group C2/c with a = 19.015(4), b = 7.7697(16), c = 15.298(3) A, β = 98.24(3)°, V = 2236.8(8) A^3, Z = 8, F(000) = 760, D_c = 1.029 mg/m^3, μ = 0.057 mm^-1, T = 293(2) K, S = 1.100, R = 0.0673 and wR = 0.1391 for 1302 observed reflections with I 〉 2σ(I).
A novel method for the synthesis of novel silalactone was proposed by iodation and zirconium-mediated cycloaddition of alkynes. 1,1-Dimethyl-4-carboxylatethyl-6,7-diphenyl-5-(trimethylsilyl)-1,3-dihydrobenzo[c][1,2]oxasilol-3(1 H)-one(compound 1) was obtained and characterized by X-ray single-crystal diffraction. It belongs to the monoclinic system, space group P2_1/n with a = 12.706(3), b = 10.826(2), c = 19.407(4) A, β = 91.50(3)°, V = 2668.4(9) A^3, Z = 4, F(000) = 1004, D_c = 1.182 mg/m^3, μ = 0.162 mm^-1, T = 293(2) K, S = 1.129, R = 0.0868 and wR = 0.1607 for 3542 observed reflections with I 〉 2σ(I). The butadiene derivative, 3,6-di(2-methylphenyl)-4,5-diethylocta-3,5-diene(compound 2), was synthesized by zirconacyclopentadiene and aryl iodides in the presence of Cu Cl and Pd(PPh3)4. It was characterized by X-ray single-crystal diffraction for the first time, belonging to the monoclinic system, space group C2/c with a = 19.015(4), b = 7.7697(16), c = 15.298(3) A, β = 98.24(3)°, V = 2236.8(8) A^3, Z = 8, F(000) = 760, D_c = 1.029 mg/m^3, μ = 0.057 mm^-1, T = 293(2) K, S = 1.100, R = 0.0673 and wR = 0.1391 for 1302 observed reflections with I 〉 2σ(I).