《Table 1Optimization studies.a》
本系列图表出处文件名:随高清版一同展现
《Co(Ⅲ)/Zn(Ⅱ)催化吲哚的分子内环丙烷化(英文)》
a The reaction was carried out using 1a(0.2 mmol),2a(0.24 mmol),[Cp*Co(MeCN)3][SbF 6]2(5 mol%),and Zn(OAc)2(30 mol%)in DCM(2 mL)at30–45°C for 12–24 h.b Isolated yield.c Determined by 1H NMR.
We initiated our investigation by screening the reaction conditions of the coupling of N‐pyrimidinylindole(1a)with ene‐yne ketone(2a)under Co(III)/Zn(II)catalysis(Table 1).The preliminary experimentation highlighted the effectiveness of the combined Co(III)/Zn(II)catalysis.The control experi‐ments revealed that both Co(III)and Zn(II)were important for this transformation.The omission of Co(III)resulted in trace formation of the desired product(entries 1 and 3),whereas the exclusion of Zn(II)resulted in a lower yield(entries 2 and 4).Note that the transformation proceeded in a highly regioselec‐tive manner.Neither Co(III)nor Zn(II)is effective against de‐pression when applied alone(entries 1–4).The solvent was observed to exert a dramatic impact on the efficiency.Notably,dichloromethane was identified as the optimal solvent in terms of both the yield and diastereoselectivity,for the formation of3aa(entries 5–9).Lowering the reaction temperature further resulted in low efficiency(entry 10),and extending the reaction time resulted in a yield(entry 11)approximately equal to that under the optimized reaction conditions(entry 9).
图表编号 | XD008201000 严禁用于非法目的 |
---|---|
绘制时间 | 2018.12.01 |
作者 | 李娜、常俊标、孔令恒、王栓景、王丹丹、程淼、李兴伟 |
绘制单位 | 河南师范大学化学化工学院河南省有机功能分子和药物创新重点实验室、新乡医学院药学院、河南师范大学化学化工学院河南省有机功能分子和药物创新重点实验室、中国科学院大连化学物理研究所、河南师范大学化学化工学院河南省有机功能分子和药物创新重点实验室、河南师范大学化学化工学院河南省有机功能分子和药物创新重点实验室、河南师范大学化学化工学院河南省有机功能分子和药物创新重点实验室、河南师范大学化学化工学院河南省有机功能分子和药物创新重点实验室、中国科学院大连化学物理研究所 |
更多格式 | 高清、无水印(增值服务) |