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]...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）.展开更多
文摘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）.
