Diethyl ether (distilled from NaK_2.2)
Neopentyl lithium (see [[120|Page 120]])
Zirconium tetrachloride (Aldrich)

To a large schlenk tube with stirrer bar charged with ZrCl₄ (2.00 g, 8.58 mmol) and diethyl ether (50 ml) at -78^oC (acetone / dry ice) was added dropwise a solution of LiCH₂CMe₃ (2.70 g, 37.95 mmol) in diethyl ether (50 ml) over a period of 40 min in the absence of light and with vigorous stirring. After complete addition, the reaction mixture was then surrounded with dry ice (which gradually evaporates)and was stirred overnight. The mixture had turned brown and a precipitate had formed (presumably LiCl). The mixture was then concentrated in vacuo to ca. 5 ml, transfered to a sublimation device. All volatiles were then removed and the system was attached to a turbo pump. The mixture was sublimated at 85^oC (by heating the sublimation tube inside a horizontal furnace), 10^-6 mm Hg, to yield an off-white solid. Yield = 2.41 g, 75 %.

¹H NMR (d₆ benzene) 1.45 (s, 2H, CH₂), 1.21 (s, 9H, CMe₃).

P. J. Davidson et al, J. Orgaomet., Chem., 57, 1973, 269