in benzene dropwise addn. of soln. of TiCl4 to soln. of Li-compd. (under Ar or N2)for 30 min, stirring overnight; filtn., washing with benzene, drying;

C5H5SiMe3; C4H9Li in tetrahydrofuran; hexane under N2; adding 2.5 M nBuLi in hexane to THF soln. of C5H5SiMe3 at -70°C, stirring for 5 min, warming within 1 h to 25°C, heatingto reflux for 5 min, cooling to 25°C, adding THF soln. of (C5H5) TiCl3, heating to reflux for 1 h; removal of volatiles in oil pump vac., extg. residue with CH2Cl2, filtering through SiO2, removal of solvents in oil pump vac.; elem. anal.;

(n)BuLi in diethyl ether; hexane byproducts: LiCl, Me2S; N2-atmosphere; stirring equimolar amts. of BuLi and alkyne at 0°C, addn. of Au-complex, stirring for 30 min, addn. of Ti-complex, stirring for 2 h at 25°C; evapn., extn. (pentane), filtration (Celite), concn., cooling (0°C); elem. anal.;

in tetrahydrofuran byproducts: Cu; under N2; soln. of Ti-Fe complex in THF at -10°C mixed with CuCl2 (molar ratio 1:1.07) in THF; stirred at -10°C for 30 min; volatiles removed in vac.; sepd. by chromy. (Kieselgur, -30°C, n-pentane); eluted with Et2O (Fe complex) and THF (Ti complex);

in tetrahydrofuran byproducts: Pd; under N2; PdCl2 in THF reacted with equimolar amt. of Ti complex in THFfor 3 h at 25°C; filtered through Kieselgur; volatiles removed in vac.; sepd. by chromy.(Kieselgel, -20°C, n-pentane); eluted with n-pentane (Me3SiC4SiMe3) and CH2Cl2 (Ti complex);

in diethyl ether; water byproducts: HOCH2CCCH3; N2 atm.; 25°C;

in dichloromethane; water N2 atm.; stirring (1 h, 25°C); evapn. (vac.), filtn. (SiO2/Et2O, 25°C); elem. anal.;

in tetrahydrofuran byproducts: FeCl2; under N2; mixt. of FeCl3 and Ti complex (molar ratio 1:1) in THF stirred at 25°C for 1 h; volatiles removed in vac.; extd. with n-pentane; fractionary crystn. from THF-n-pentane at -30°C; detd. by elem. anal., IR, NMR, and mass spectroscopy;

in tetrahydrofuran byproducts: (CuCl)(n); under N2; soln. of CuCl2 in THF at 25°C mixed with equimolar amt. of Ti complex in THF; stirred at 25°C for 2 h; filtered through Kieselgur; volatiles removed in vac.; sepd. by chromy.(Kieselgel, -20°C, n-pentane);

in tetrahydrofuran byproducts: (CuCl)(n); under N2; soln. of CuCl2 in THF at 25°C mixed with equimolar amt. of Ti complex in THF; stirred at 25°C for 2 h; filtered through Kieselgur; volatiles removed in vac.; sepd. by chromy.(Kieselgel, -20°C, n-pentane);