in diethyl ether; benzene byproducts: (C6F5)2GeBr2, (C6F5)3GeBr; GeCl4 in benzene added to etheric soln. of C6F5MgBr; driving off ether and replacing by more C6F6; refluxing for 10 h;
magnesium in toluene byproducts: MgBrCl; (Ar); treatment of o-BrC6H4OCH3 with Mg in toluene; reflux with GeCl4 for 30 h; treatment with satd. aq. NH4Cl; extn. of aq. layer with THF; drying of combined extracts over MgSO4; removal of THF (vac.); recrystn. twice fromEtOH or MeCN; elem. anal.;
参考文献
Yoder, Claude H.; Agee, Tamara M.; Griffith, Allison K.; Schaeffer Jr., Charles D.; Carroll, Mary J.; Detoma, Alaina S.; Fleisher, Adam J.; Gettel, Cameron J.; Rheingold, Arnold L.
Organometallics, 2010 , vol. 29, # 3 p. 582 - 590
aluminium trichloride in cyclohexane other Radiation; a mixt. of GeCl4 and tetraphenylgermane in presence of AlCl3 as catalyst in cyclohexane in a Pyrex tube is irradiated with a light stream of argon for 20 min at atmospheric pressure (microwave irradiation: 300 W) (Ar); identification by (1)H-NMR, gas chromy.;
参考文献
Laurent, Regis; Laporterie, Andre; Dubac, Jacques; Berlan, Jacques
Organometallics, 1994 , vol. 13, p. 2493 - 2495
in melt according to F. Rijkens, G.J.M. van der Kerk, Rec. Trav. Chim. 83 (1964)723; under dry O2-free Ar using Schlenk techniques; mixt. of Ph4Ge (5.35mmol), AlCl3 (0.49 mmol) and GeCl4 (1.60 mmol) heated (120°C, 4 h); cooled to room temp.; recrystd. from hexane;
参考文献
Zaitsev, Kirill V.; Kapranov, Andrey A.; Oprunenko, Yuri F.; Churakov, Andrei V.; Howard, Judith A.K.; Tarasevich, Boris N.; Karlov, Sergey S.; Zaitseva, Galina S.
Journal of Organometallic Chemistry, 2012 , vol. 700, p. 207 - 213
