tetrachloromethane in tetrachloromethane byproducts: CCl3; Irradiation (UV/VIS); Irradiation λ >350 nm, CCl4, Ar atm.;; detected by IR spectra and GCA;;
参考文献
Goldman, Alan S.; Tyler, David R.
Organometallics, 1984 , vol. 3, p. 449 - 456
Na#Hg in tetrahydrofuran Mn2(CO)10 was treated with sodium amalgam (room temp., N2, 45 min); after removing of amalgam Re complex soln. was added dropwise (30 min); evapn., sublimation;
CO in n-heptane Mn2(CO)10 (15 mg, 0.045 mmol) and (η3-CPh3)Re(CO)4 (52 mg, 0.09 mmol) dissolved in 20 ml heptane, solution was degassed and stirred over 18 h under CO (20 psi);; detected by IR;;
参考文献
Crocker, Lisa S.; Mattson, Bruce M.; Heinekey, D. Michael; Schulte, Gayle K.
Inorganic Chemistry, 1988 , vol. 27, p. 3722 - 3725
sodium amalgam in tetrahydrofuran (Ar), reduced Mn-complex (45 min at 0°C, 30 min at 20°C) added at -70°C, stirred for 1 h; solvent removed in vacuo at -30°C, extracted four times with pentane at -25°C (Mn2(CO)10 as by-product), extracted two times with CH2Cl2, solvent removed, dried in high vacuum, (all steps at <-20°C), elem. anal.;
