Synthesis
Titanium(III) chloride tetrahydrofuran complex was prepared as follows: to a 2L round-bottomed flask (fitted with a thermometer, mechanical stirrer and reflux condenser) was added granulated titanium (~100 mesh, 99.9 purity, 8.3 g), titanium tetrachloride (98.6 g) and toluene (800 g). THF (432 g) was added under ice cooling while maintaining the tank temperature at 10-20 C. The reaction mixture was heated to reflux (90-100 C) for 6 hours. The reaction mixture was then cooled to room temperature and filtered. The solid tetrahydrofuran titanium chloride product was washed with deoxyhexane (200 mL) and dried under vacuum, yield = 240 g; 94%, based on the total charge of titanium (TiCl4 and particulate titanium).
