n-butyllithium in diethyl ether; hexane (N2); addn. dropwise of soln. of n-BuLi/hexanes at -75°C for 0.5 h to stirred soln. of propyne in Et2O; stirring for 1.5 h at -75°C; addn. dropwise soln. of (i-Pr)OBO2C2Me4 in Et2O for 1 h; warming to 20°C for 4 h; stirring for 16 h; addn. of HCl soln. in Et2O at 0°C for 45 min; stirring for 0.5h at 0°C and for 1.5h at 20°C; pptn., filtration, washing with hexane; combining of org. solns., removal of solvent under reduced pressure, fractional distn., elem. anal.;

暂无反应条件数据

1.1: Schwartz's reagent / tetrahydrofuran / 1 h / 20 °C / |Inert atmosphere 1.2: 1 h / 20 °C / |Inert atmosphere 2.1: hydrogen; [Ir((S)-PPh2C6H4C3H3NOiPr)(COD)](tetrakis(3,5-di(trifluoromethyl)phenyl)borate) / dichloromethane / 18 h / 50 °C / 22502.3 Torr View Scheme

1.1: Schwartz's reagent / dichloromethane / 1 h / 20 °C / Inert atmosphere 1.2: Inert atmosphere 2.1: (η-1,5-cyclooctadiene) {[4(R),5(R)]-1-benzoyl-2-[(S)-2-diphenylphosphinoferrocenyl]-4,5-diphenyl-4,5-dihydro-1-imidazole} iridium(I) tetrakis[3,5-bis(trifluoromethyl)phenyl]borate; hydrogen / dichloromethane / 18 h / 50 °C / 3750.38 Torr View Scheme

1.1: Schwartz's reagent / tetrahydrofuran / 1 h / 20 °C / |Inert atmosphere 1.2: 1 h / 20 °C / |Inert atmosphere 2.1: (cyclooctadiene)((3,5-dimethylphenyl)2PCH2C(CH3)2(C3H3NO)(tBu))Ir(tetrakis(3,5-(trifluoromethyl)phenyl)borate); hydrogen / dichloromethane / 18 h / 50 °C / 22502.3 Torr View Scheme