in neat (no solvent)
thermal decompn. of PhBClNt-BuSiMe3 at 575°C and 0.005 Torr; products condensed at -196°C; reaction mixt. liquefies at ca. -60°C; removal of Me3SiCl at -45°C;
参考文献
Bonn, Karl-Heinz van; Bennigsen-Mackiewicz, Theo von; Kiesgen, Jutta; Plotho, Christoph von; Paetzold, Peter
Zeitschrift fuer Naturforschung, B: Chemical Sciences, 1988 , vol. 43, # 1 p. 61 - 68
in neat (no solvent)
Schlenk techniques used; dry oxygen-free nitrogen or argon atm.; supension of (Nb(η5-C5H4Si(CH3)3)2Cl2)PF6 in Me3SiOCH2CH3; stirring (3 h/room temp.); initial red solid turns yellow;; filtration; washing (hexane); recrystn. (dissolving in chloroform/overlayered by hexane/few days); elem anal.;;
in neat (no solvent)
Schlenk techniques used; dry oxygen-free nitrogen or argon atm.; supension of (Nb(η5-C5H4Si(CH3)3)2Cl2)PF6 in Me3SiOCH(CH3)2; stirring (3 h/room temp.); initial red solid turns yellow;; filtration; washing (hexane); recrystn. (dissolving in chloroform/overlayered by hexane/few days); elem anal.;;
tetrachloromethane in cyclohexane
Irradiation (UV/VIS); irradiation of catenate in cyclohexane containing CCl4 with a 110 W low pressure Hg arc lamp at room temp. under Ar for 1-4 h; identification by GC and GC-MS;
参考文献
Mochida, Kunio; Kikkawa, Haruhiko; Nakadaira, Yasuhiro
Journal of Organometallic Chemistry, 1991 , vol. 412, # 1.2 p. 9 - 19
CH2Cl2 in dichloromethane
CH2Cl2 (-78°C) added to cold (-78°C) mixt. of Nb complex and (Cp2Fe)PF6 in 2:1 molar ratio under inert atm., cold bath removed, allowed to stir for 3 h; volatiles removed, extd. with Et2O, evapn. of ext. gave Cp2Fe (NMR); residue extd. with acetone, quickly filtered, pumped, washed with Et2O to give (Cp2Nb(CH2SiMe3)Cl)PF6 (NMR); remaining powder identified by IR to be Cp2NbCl2; Me3SiHal identified by GC;
参考文献
Arnold, John; Tilley, T. Don; Rheingold, Arnold L.; Geib, Steven J.
Organometallics, 1987 , vol. 6, p. 473 - 479
thionyl chloride
byproducts: SO2; ratio of (CH3)2SbOSi(CH3)3 and SOCl2 1:2, freezing with liq. air, then warming up; seprd. by fractionation;
参考文献
Schmidbaur, H.; Arnold, H. S.; Beinhofer, E.
Chemische Berichte, 1964 , vol. 97, p. 449 - 458
Full Text Show Details
Gmelin Handbook: Sb: Org.Comp.2, 1.2.1.1.9.6, page 34 - 35
Zheltonogova, E. A.; Orlova, N. A.; Kobzareva, V. P.; Shipov, A. G.; Baukov, Yu. I.
J. Gen. Chem. USSR (Engl. Transl.), 1991 , vol. 61, # 10 p. 2254 - 2262,2092 - 2099
