in hexane; cyclohexane 1-bromooctane (1 equiv.) and TMTH (2 equiv.) in hexane cooled to 0°C under Ar, LDA (1 equiv., 1.6 M soln. in cyclohexane) dropped in, stirred for 20-25 min at room temp., quenched with water; analyzed by GC (after quenching), NMR (before quenching);
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;
Ren, Peng; Vechorkin, Oleg; Von Allmen, Kim; Scopelliti, Rosario; Hu, Xile
Journal of the American Chemical Society, 2011 , vol. 133, # 18 p. 7084 - 7095
