HCID 70012514, compound → HCID 178504157, compound

Participants

Reaction Steps

5 g (19.03 mmol) of cyclopentadienylzirconium trichloride (CpZrCl3) was placed into a flask with 20 mL of dichloromethane to form suspension. 3.92 g (19.03 mmol) of lithium 1-(1-methyl-1-silacyclobutyl)indene was also placed into another flask with 20 mL of dichloromethane to form suspension. The suspension of CpZrCl3 in the first flask was slowly added into the suspension of lithium 1-(1-methyl-1-silacyclobutyl)indene in the second flask, and then the remained reactant in the first flask was washed with 10 mL of dichloromethane and added into the second flask. After repeating the washing and addition process for three times, the reaction mixture was stirred overnight. After the completion of reaction, LiCl was filtered and removed from the formed yellowish solution with 11G4 filter. The solvent was then evaporated from the filtrate under vacuum and the remaining volatile material was also removed under vacuum at 50° C. overnight. The concentrate was then sublimated at 130° C. in the presence of 50μ Hg to obtain 5.85 g (72% of yield) of pure ((1-methyl-1-silacyclobutyl)-indenyl)(cyclopentadienyl)zirconium dichloride having the following 1H NMR (CDCl3, ppm) data: δ7.95 (d, 1H), 7.92 (d, 1H), 7.42-7.28 (m, 2H), 7.14 (d, 1H), 6.84 (d, 1H), 6.10 (s, 5H, C5H5), 2.38-2.15 (m, 2H), 1.57-1.27 (m, 4H), 0.74 (s, 3H).

Provenance & Evidence