water in tetrahydrofuran; hexane under N2 atm.; Teflon valved NMR tube was loaded with Fe complex; soln. of n-BuLi in hexane was added; THF added; NMR tube was shaken for several min; volatiles removed (vac.); solid dissolved in C6D6; DMF condensed into NMR tube; mixt. was shaken; H2O added; monitored by NMR spectroscopy;
参考文献
Meijboom, Reinout; Beagley, Paul; Moss, John R.; Roodt, Andreas
Journal of Organometallic Chemistry, 2006 , vol. 691, # 5 p. 916 - 920
water in tetrahydrofuran; hexane under N2 atm.; Teflon valved NMR tube was loaded with Fe complex; soln. of n-BuLi in hexane was added; THF added; NMR tube was shaken for several min; volatiles removed (vac.); solid dissolved in C6D6; DMF condensed into NMR tube; mixt. was shaken; H2O added; monitored by NMR spectroscopy;
参考文献
Meijboom, Reinout; Beagley, Paul; Moss, John R.; Roodt, Andreas
Journal of Organometallic Chemistry, 2006 , vol. 691, # 5 p. 916 - 920
in tetrahydrofuran byproducts: Si(CH2CH2CH2SiMe2CH2Li)4; (N2 or Ar); using Schlenk techniques; treatment of Si(CH2CH2CH2SiMe2CH2SnBu3)4 with 4.0 equiv. of BuLi at 0°C for 30 min; evapn. of solvent, extn. with pentane;
参考文献
Meijboom, Reinout; Hutton, Alan T.; Moss, John R.
Organometallics, 2003 , vol. 22, # 9 p. 1811 - 1815
in tetrahydrofuran; hexane under N2 atm.; soln. of n-BuLi in hexane was added to soln. of complex in THF at -78°C in H-type Schlenk tube; mixt. stirred for 30 min at -78°C; several drops of BuLi in hexane were added; volatiles evapd. (vac.); pentane distd. onto mixt.; mixt. was stripped with pentane by distg. pentane onto the mixt. and evapg. in vac.; mixt. washed (pentane); volatiles removed (vac.);
参考文献
Meijboom, Reinout; Beagley, Paul; Moss, John R.; Roodt, Andreas
Journal of Organometallic Chemistry, 2006 , vol. 691, # 5 p. 916 - 920