in toluene mixing of soln. of (C5Me5)TiMe(O(t-Bu))2 and AlMe3 (2 equiv.) in toluenein sealed ampule; heating to 100°C for 1 h; evapn. of all volatiles on vac. line at 60°C; condensing to activated charcoal colled with liq. N2; dissolving in C6D6 or C7D8; pouring into NMR tube; sealing; monitoring by NMR;