in tetrahydrofuran 48 h; Schlenk techniqueInert atmosphere;

n-butyl lithium in hexane; toluene Cp'H (erlenmeyer flask), adding n-butyl lithium/hexane (stirring 10 min); adding solid ZrCl4 (N2-atmosphere), stirring; heating to reflux 48 h; cooling; removing of volatiles; residue adding to CH2Cl2; extracting with 4N HCl (green solution); stripping of volatiles; recrystn. (toluene); sublimation of residue for additional product;

C5H5Me; BuLi; HCl in hexane; water; toluene stirring (room temp., 1 h, vac.), ZrCl4 addn., refluxing (Ar-atmosphere), HCl (aq) addn.; filtering, recrystn. (toluene);

in tetrahydrofuran ZrCl4/NaC5H4CH3 (molar ratio: 1:2); dry THF;;

in tetrahydrofuran (N2); std. Schlenk technique; soln. of Na compd. (2 equiv.) in THF was slowly added to stirred suspn. of Zr compd. in THF at -78°C; warmed to room temp.; refluxed for 18 h; cooled; filtered; dried (vac.); sublimed (180°C, 0.1 Torr); elem.anal.;

in toluene byproducts: Sn(CH3)2Cl2; (N2); using Schlenk techniques; addn. of Me2Sn(C5H4Me-1)2 to ZrCl4 in toluene; stirring under reflux for 24 h; evapn.; addn. of hexane; filtration, concn.; cooling; crystn., elem. anal.;

in ethylene glycol dimethyl ether; toluene N2 atmosphere; addn. of soln. of org. compd. in DME to Zr-compd. in toluene, refluxing (1 h), stirring (12 h, room temp.); evapn., extn. (toluene), recrystn. (toluene);

in tetrahydrofuran byproducts: 2,6-diacetylpyridine; under Ar; MeMgCl is added to a stirred soln. of the starting complex in THF, stirred overnight; evapd. to dryness, the residue is shaken in aq. HCl/CH2Cl2, the extract is dried, evapd. in vac., detected by NMR;

methylaluminoxane in benzene-d6 under Ar, standard Schlenk techniques; solid dichloride Zr complex mixedwith 1 equiv. of Cp2ZrClMe; dissolved in benzene-d6; a minute amt. of s olid methylaluminoxane added; equil. reached within several min; not isolated; monitored by (1)H NMR spectra;