in toluene addition of MeLi to GaCl3 at -78°C; solution was added to NaN3 in toluene at -78°C; stirring; was allowed to warm to room temperature; heating under reflux for 18h; solvent was removed under vacuum; sublimation (58°C, 1E-3 Torr);
参考文献
Atwood, Jerry L.; Jones, Richard A.; Cowley, Alan H.; Atwood, Jerry L.; Bott, Simon G.
Journal of Organometallic Chemistry, 1990 , vol. 394, # 1/3 p. C6 - C8
in tetrahydrofuran TMTH (1.10 mmol) and 1-bromooctane (1.10 mmol) in THF cooled to 0°C under Ar, MeLi (1.10 mmol) in THF added, stirred for 15 min at room temp., hydrolyzed with water; H2 collected with gas measuring device, GC analysis of org. layer;
in diethyl ether TMTH (1.00 mmol) and 1-bromooctane (1.00 mmol) in Et2O cooled to 0°C under Ar, MeLi (1.00 mmol, 1.00 M soln. in Et2O) added, stirred for 15 min at room temp., hydrolyzed with water; H2 collected with gas measuring device, GC analysis of org. layer;
in tetrahydrofuran byproducts: methane, butane; excess MeLi, 30-50°C, ca. 1 h; Li(1+) cation in the resulting complex is solvated with 3-5 molecules of THF, trace of butenes were also detected, U-Me to U-Bu complexes ratio was 9:1 according to (1)H NMR spectral data; GC anal. of the gas. phase, (1)H NMR;
