tetrahydrofuran in tetrahydrofuran byproducts: hexamethylbenzene; Ar-atmosphere; addn. of Ti-complex to excess THF cooled to -120°C, warming to room temp.; volume reduction, cooling to -30°C (crystn. of TiCl4(THF)2 ), evapn. of soln., heptane addn., filtration of second crop of TiCl4(THF)2, volume reduction, crystn. on cooling (-30°C), decantation, drying(vac.);

in toluene byproducts: LiCl; (Ar); dropwise addn. of li salt in toluene to TiCl4 toluene soln. at -40°C, gradual warming to room temp., stirred at room temp. for 20 min; filtered, solvent removed (vac.); contaminated with TiCl4(THF)2; elem. anal.;

in dichloromethane (N2); stirring (4 h); filtration, washing (CH2Cl2), drying (vac.); elem. anal.;

germanium tetrachloride in tetrahydrofuran

in tetrahydrofuran

in tetrahydrofuran under Ar; Ti complex treated with THF; refluxed for 2 h; solvent removed in vac.; detd. by IR and (1)H NMR spectra;

in toluene (Ar); a soln. of Li-salt added slowly to a soln. of 1/2 equiv. TiCl4 at-78°C, allowed to warm to room temp., stirred for 2 h; filtered, concd., cooled overnight; inseparable;

in neat (no solvent) direct reaction between the components in a vacuum;

in toluene under N2; TiCl4(thf)2 added in small portions to soln. of LiNEt2 in toluene, stirred overnight at room temp., heated at 100°C for severalhours; toluene replaced with pentane, soln. filtered, extd. before the solvent was removed, dried under vac.;

in not given under Ar or N2, prepn. in accordance with the method of Bradley and Thomas (J. Chem. Soc. (London) (1960), 3857), except TiCl4(THF)2 employed instead of TiCl4 and react. carried out at room temp.;