The title complex,(1S)-1,1'-bis{[N-ethyl-N-(1-methylethyl)-amino]carbonyl}-2-(hydroxyldiphenylmethyl)-ferrocene([Fe(C_(24)H_(22)NO_(2))(C_(11)H_(16)NO)]_(2)·H_(2)O,Mr=1207.13),was synthesized via(-)-Sparteine...The title complex,(1S)-1,1'-bis{[N-ethyl-N-(1-methylethyl)-amino]carbonyl}-2-(hydroxyldiphenylmethyl)-ferrocene([Fe(C_(24)H_(22)NO_(2))(C_(11)H_(16)NO)]_(2)·H_(2)O,Mr=1207.13),was synthesized via(-)-Sparteine-mediated enantioselective directed ortho-lithiation of 1,1‘-bis{[N-ethyl-N-(1-methylethyl)-amino]carbonyl}-2-(hydroxydiphenylmethyl)-ferrocene.The structure of the rifle compound was determined by X-ray single-crystal diffraction.The crystal belongs to the orthorhombic system,space group P2_(1)2_(1)2_(1),with a=10.266(2),b=17.676(4),c=34.097(7)A,V=6187(2)A3,Z=4,C_(70)H_(86)Fe_(2)N_(4)O_(7),Dc=1.296 g/cm^(3),μ=0.527 mm^(-1),T=113(2)K,F(000)=2568,the final R=0.0469 and wR=0.0984 for 13940 observed reflections with I〉2σ(I).The neighboring ferrocene derivatives are joined into dimers via O-H…O=C intermolecular hydrogen bonding by a water molecule.Besides,the dimers form neat rows along the a axis.展开更多
乙酸(1-二茂铁基乙基)酯(记为配体2)与1-异丙基咪唑经过季铵化反应,制备出具有大空间位阻和富电子的配体1-(1-二茂铁基乙基)-3-异丙基-1-咪唑碘盐(记为配体1),收率为88%。利用1 H NMR、13 C NMR对其结构进行了表征,并进一步考察了体系Pd...乙酸(1-二茂铁基乙基)酯(记为配体2)与1-异丙基咪唑经过季铵化反应,制备出具有大空间位阻和富电子的配体1-(1-二茂铁基乙基)-3-异丙基-1-咪唑碘盐(记为配体1),收率为88%。利用1 H NMR、13 C NMR对其结构进行了表征,并进一步考察了体系Pd(OAc)2/配体1催化4-甲氧基溴苯与苯硼酸的Suzuki-Miyaura偶联反应活性。实验发现:配体1在催化反应过程中可以有效地稳定Pd,在二氧六环反应介质中,碳酸铯为碱,1%Pd用量的条件下可以有效催化Suzuki-Miyaura偶联反应,加热回流3h,收率达93%。展开更多
基金supported by the Major Program of National Natural Science Foundation of China(200572009)Beijing Natural Science Foundation Program and Scientific Research Key Program of Beijing Municipal Commission of Education(KZ200610011006)
文摘The title complex,(1S)-1,1'-bis{[N-ethyl-N-(1-methylethyl)-amino]carbonyl}-2-(hydroxyldiphenylmethyl)-ferrocene([Fe(C_(24)H_(22)NO_(2))(C_(11)H_(16)NO)]_(2)·H_(2)O,Mr=1207.13),was synthesized via(-)-Sparteine-mediated enantioselective directed ortho-lithiation of 1,1‘-bis{[N-ethyl-N-(1-methylethyl)-amino]carbonyl}-2-(hydroxydiphenylmethyl)-ferrocene.The structure of the rifle compound was determined by X-ray single-crystal diffraction.The crystal belongs to the orthorhombic system,space group P2_(1)2_(1)2_(1),with a=10.266(2),b=17.676(4),c=34.097(7)A,V=6187(2)A3,Z=4,C_(70)H_(86)Fe_(2)N_(4)O_(7),Dc=1.296 g/cm^(3),μ=0.527 mm^(-1),T=113(2)K,F(000)=2568,the final R=0.0469 and wR=0.0984 for 13940 observed reflections with I〉2σ(I).The neighboring ferrocene derivatives are joined into dimers via O-H…O=C intermolecular hydrogen bonding by a water molecule.Besides,the dimers form neat rows along the a axis.
文摘乙酸(1-二茂铁基乙基)酯(记为配体2)与1-异丙基咪唑经过季铵化反应,制备出具有大空间位阻和富电子的配体1-(1-二茂铁基乙基)-3-异丙基-1-咪唑碘盐(记为配体1),收率为88%。利用1 H NMR、13 C NMR对其结构进行了表征,并进一步考察了体系Pd(OAc)2/配体1催化4-甲氧基溴苯与苯硼酸的Suzuki-Miyaura偶联反应活性。实验发现:配体1在催化反应过程中可以有效地稳定Pd,在二氧六环反应介质中,碳酸铯为碱,1%Pd用量的条件下可以有效催化Suzuki-Miyaura偶联反应,加热回流3h,收率达93%。
