Tetrachlorobis tetrahydrofuran zirconium IV , ZrCl4 thf

The product is a white, crystalline solid which is air sensitive. It melts with decomposition at 170-171°. Its infrared spectrum contains a sharp, strong peak at 990 cm 1 and a strong, broad peak at 820-840 cm 1. 

TETRACHLOROBIS(TETRAHYDROFURAN)HAFNIUM(IV), HfCl4(thf)2 HfCl4 + 20C4H8------------------- HfCl4(OC4H8)2 

A 500-mL, single-neck, round-bottom flask equipped with a reflux condenser and magnetic stirring bar is charged with 200 mL anhydrous tetrahydrofuran and 10.0 g (65mmole) titanium trichloride. The solution is heated to reflux for 22 hours, then allowed to cool to room temperature. The resulting pale-blue crystals are collected on a medium fritted funnel and washed with 50 mL dry pentane. The pentane wash plus another 50 mL dry pentane are added to the mother liquor to give a second crop of pale-blue solids. The total yield is 21.96 g (91.4%). 

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