Hexakis 2-trifluoromethyl-2-propoxy dimolybdenum III

Under a N2 atmosphere, a 100 mL round-bottomed flask containing a Teflon-coated stir bar is charged sequentially with THF (50 mL) and WCI4 (5.377 g, 

5 mmol). The resulting suspension is frozen solid in liquid nitrogen and allowed to thaw over a magnetic stir plate. As soon as the suspension has melted sufficiently that stirring begins, sodium amalgam (0.38 g Na in 7mL of Hg  

The checkers note that this preparation often affords lower yields if carried out on smaller scale. The checkers added the sodium amalgam in three portions over 30 min from a dropping funnel under argon. 

NaW2Cl7(THF)5 -I- 6NaO-t-Bu WzCO-t-Bu) 4- 7NaCl 4- 5THF Procedure 

Under a N2 atmosphere, a 100 mL round-bottomed flask containing a Teflon-coated stir bar is charged with NaW2Cl7(THF)5 (1.00 g, 1.01 mmol) and THF (40 mL). The resulting green solution is cooled to -35°C, and then is treated with NaO-f-Bu (0.580 g, 6.03 mmol). The reaction mixture is stirred for 18 h at ambient 

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