Lithium, mol. (Li2) → HCID 131723810, compound

Participants

Reaction Steps

The previously distilled ligand (20.2 g, 0.07 mol) was placed in a 500 ml Schlenk flask and dissolved in dry hexane (250 ml). n-BuLi 1.6 M in hexane (87.3 ml 0.14 mol) was dropwise added is solution at 5° C. The resulting white suspension was heated to 75° C. for a 6 h period until the total formation of the dilithium salt was confirmed by NMR. The mixture was left to cool down to room temperature, filtered and dried under vacuum. ZrCl4 (16.28 g, 0.07 mol) was placed in the 500 Schlenk flask and toluene (200 ml) was added, and, at the same time, toluene (200 ml) was added to 2,2-bis(cyclopentadienyl)-5trimethylsiloxypentane dilithium salt. Both suspensions were cooled to −78° C. and the dilithium salt slurry was, via cannula, added to the ZrCl4 one. The resulting off-white suspension was allowed to warm to room temperature and stirred for 16 h. The resulting orange-red suspension was filtered and the cake washed with toluene (100 ml). The solvent was removed under vacuum and the resulting oily solid was repeatedly extracted with hexane, concentrated to 1/10 in volume and cooled to −30° C. to afford yellow crystals of the product (6.8 g, 22% yield). 1H NMR (CDCl3): Λ6.70 (C5H4, d, 4H), 5.82 (C5H4, d, 4), 3.75 (CH2, t, 2H), 2.28 (CH2, m, 2H), 1.83 (CH2, m, 2H), 1.80 (CH3, s, 3H), 0.18 ((CH3)3, s, 9H).

Provenance & Evidence