以对叔丁基苯酚为原料,经一步法制得对叔丁基杯[6]芳烃。通过逆傅克反应、亲核取代反应制得二烷基化杯[6]芳烃。最后通过磺化、亲核取代等反应,合成了下缘含喹啉基长链的新型夹状醚杯[6]芳烃化合物( 2a~ 2c ),其结构经 1 H NMR, 13 C NM...以对叔丁基苯酚为原料,经一步法制得对叔丁基杯[6]芳烃。通过逆傅克反应、亲核取代反应制得二烷基化杯[6]芳烃。最后通过磺化、亲核取代等反应,合成了下缘含喹啉基长链的新型夹状醚杯[6]芳烃化合物( 2a~ 2c ),其结构经 1 H NMR, 13 C NMR和HR-MS(ESI-QTOF)表征。以10.0 mol%杯[6]芳烃化合物( 2b )为相转移催化剂,20.0 mol%KOH为催化剂,THF为溶剂,较高产率和高选择性地合成了一系列( Z )-1,2-二芳硒基烯化合物,其结构经 1 H NMR和NOESY确证。 2b 重复使用6次,催化活性无明显降低。展开更多
A new series of quinoxalinophenazine derivatives were synthesized in good yields by the reaction of 2,3-dibromonaphthalene-1,4-dione with different aryl-1,2-diamines in DMF as solvent at 120-130℃ or under reflux cond...A new series of quinoxalinophenazine derivatives were synthesized in good yields by the reaction of 2,3-dibromonaphthalene-1,4-dione with different aryl-1,2-diamines in DMF as solvent at 120-130℃ or under reflux conditions. 3,12-dimethylbenzo[a]quinoxalino[2,3-c] phenazine with bidentate character reacts with mercury（II） bromide to give suitable crystals. All products were confirmed by IR, ^1H and ^13C NMR, and the metal complex by single-crystal X-ray method. The crystal（C24H16Br2HgN4, Mr = 720.82） belongs to the triclinic system, space group P1 with a = 10.186（6）, b = 10.421（6）, c = 11.470（7） A, α = 98.670（7）, β = 95.069（7）, γ = 109.831（7）°, V = 1119.4（12） A3, Z = 2, Dc = 2.139 Mg/m^3, μ = 10.46 mm^-1, F（000） = 676, R = 0.043 and wR = 0.115 for 3982 observed reflections with I 〉 2σ（I）.展开更多
Using a catalytic amount of Nal and a stoichiometric oxidant Oxone-@,a convenient procedure has been developed for the catalytic oxidative 1,2-shift of arylalkenes in CH3CN/H2O at room temperature,which provides the c...Using a catalytic amount of Nal and a stoichiometric oxidant Oxone-@,a convenient procedure has been developed for the catalytic oxidative 1,2-shift of arylalkenes in CH3CN/H2O at room temperature,which provides the corresponding α-aryl ketones in moderate to good yields.In this protocol,sodium iodide is first oxidized into hypoiodous acid,which reacts with arylalkene to afford iodohydrin.Then,the iodohydrin is transformed into the α-aryl ketone via an oxidative 1,2-shift rearrangement.展开更多
文摘A new series of quinoxalinophenazine derivatives were synthesized in good yields by the reaction of 2,3-dibromonaphthalene-1,4-dione with different aryl-1,2-diamines in DMF as solvent at 120-130℃ or under reflux conditions. 3,12-dimethylbenzo[a]quinoxalino[2,3-c] phenazine with bidentate character reacts with mercury（II） bromide to give suitable crystals. All products were confirmed by IR, ^1H and ^13C NMR, and the metal complex by single-crystal X-ray method. The crystal（C24H16Br2HgN4, Mr = 720.82） belongs to the triclinic system, space group P1 with a = 10.186（6）, b = 10.421（6）, c = 11.470（7） A, α = 98.670（7）, β = 95.069（7）, γ = 109.831（7）°, V = 1119.4（12） A3, Z = 2, Dc = 2.139 Mg/m^3, μ = 10.46 mm^-1, F（000） = 676, R = 0.043 and wR = 0.115 for 3982 observed reflections with I 〉 2σ（I）.
基金Financial support from the National Natural Science Foundation of China(No.21072176) is greatly appreciated
文摘Using a catalytic amount of Nal and a stoichiometric oxidant Oxone-@,a convenient procedure has been developed for the catalytic oxidative 1,2-shift of arylalkenes in CH3CN/H2O at room temperature,which provides the corresponding α-aryl ketones in moderate to good yields.In this protocol,sodium iodide is first oxidized into hypoiodous acid,which reacts with arylalkene to afford iodohydrin.Then,the iodohydrin is transformed into the α-aryl ketone via an oxidative 1,2-shift rearrangement.
