magnesium; methyl iodide in tetrahydrofuran
THF soln. of ArBr was added dropwise to Mg metal, reaction was initiated with MeI, stirred for 2 h at 25°C under Ar, a soln. of Me3GeCl in THF was added dropwise, mixt. was refluxed for 2 h; cooled, treated with 5percent aq. NH4Cl, extd. with CH2Cl2, ext. was washed with water, dried (Na2SO4), fractionated; elem. anal.;
参考文献
Moerlein, S. M.
Journal of Organometallic Chemistry, 1987 , vol. 319, p. 29 - 40
methyl iodide in ammonia
Irradiation (UV/VIS); condensation of sodium-dried ammonia into round-bottomed Pyrex flask, addn. of Me3SnCl and Na, addn. of CH3OC6H4NMe3I; irradn. with stirring for30 min, quenching by addn. of MeI in excess; evapn. of ammonia, treatment with water, extn. with ether;
参考文献
Chopa, Alicia B.; Lockhart, Maria T.; Silbestri, Gustavo
Organometallics, 2001 , vol. 20, # 15 p. 3358 - 3360
sodium in ammonia
Irradiation (UV/VIS); (CH3)3SnCl was dissolved in ammonia, Na metal was added until a blue color persisted for 5 min, when the blue color dissapeared, phosphate esterwas added, the mixt. was UV-irradiated with stirring for 1 h; excess of CH3I was added, NH3 was evapd., the residue was treated with water, extd. with ether, washed with aq. satd. soln. of NaCl, dried over MgSO4, recrystd. in ethanol;
参考文献
Chopa, Alicia B.; Lockhart, Maria T.; Dorn, Viviana B.
Organometallics, 2002 , vol. 21, # 7 p. 1425 - 1429
sodium; tert-butyl alcohol in ammonia
Irradiation (UV/VIS); N2-atmosphere; portionwise addn. of Na to Sn-compd., standing for 20-30 min, addn. of t-BuOH and chloroanisole, irradiation (350 nm, 60 min); addn. of excess NH4NO3 and Et2O, evapn. of NH3, water addn., extn. of aq. layer (Et2O), drying of combined org. layers (Na2SO4), TLC (SiO2, petroleum ether);
参考文献
Yammal, Carlos C.; Podesta, Julio C.; Rossi, Roberto A.
Journal of Organometallic Chemistry, 1996 , vol. 509, # 1 p. 1 - 8
