in diethyl ether byproducts: LiCl; an abs. etheric soln. of ClTi(OCHMe2)3 was stirred at -40°C under N2, then CH3Li was added and the mixt. allowed to warm up to room temp. within 1.5 h;; after evapn. of the solvent in vac., the product was distd. directly from the residual LiCl at 48-53°C and 0.01 Torr;;
in diethyl ether byproducts: LiCl; an abs. etheric soln. of Ti(OCHMe2)4 was treated with TiCl4 under N2 at 0°C, stirred at room temp. for 1.5 h, then CH3Li was added after cooling to -30°C, stirred for another hour while warming up to room temp.;; after evapn. of the solvent in vac., the product was directly distd from the residual LiCl at 48-53°C and 0.01 Torr;;
in benzene-d6 under inert atmosphere, standard Schlenk techniques; equimolar amt. of Ti compd. and ZnMe2 mixed in C6D6; not isolated; detd. by (1)H NMR spectra;
参考文献
Journal of the American Chemical Society, , vol. 124, # 35 p. 10336 - 10348
