Addition of tetrahydrofuran to titanium tetrachlorideAddition of tetrahydrofuran to titanium tetrachloride
SyntheticPage 617
Published Jul 15, 2013
A Schlenk vessel with stirrer bar was charged with dichloromethane (30 ml) and titanium tetrachloride (2.9 ml, 26.4 mmol). The solution was stirred vigorously and THF (9 ml, 111.1 mmol) was added dropwise over 1 h. The solution was stirred for a further 20 m. Pentane (60 ml) was added, and then the solution was cooled to –30 ºC and kept overnight to yield a bright yellow crystalline solid. This was recovered by filtration and dried in vacuo, yielding [TiCl4(THF)2] (8.1 g, 92 %).