反应详情

To a manila-pink suspension of tetramethylcyclopentadienyl)zirconium trichloride, (Me4Cp)ZrCl3, (5.00 g, 15.7 mmol, 1.00 equiv.) in ether (100 mL) was added lithium indenide (1.91 g, 15.6 mmol, 1.00 equiv.). The reaction turned light, creamy yellow and became thick with precipitate. The mixture was stirred 17 hours and then evaporated in vacuo, leaving light yellow solid. The solid was extracted with dichloromethane (100 mL, then 3×10 mL) and the extracts were filtered to give beige solid and a yellow solution. The solution was evaporated in vacuo, leaving fluffy yellow solid. The solid was washed with pentane (2×20 mL) and dried in vacuo. Yield 5.88 g (94%). 1H NMR(CD2Cl2): δ 1.93 (s, 12H, Me), 5.86 (s, 1H, Cp-H), 6.36 (d, 2H, Ind-H), 6.67 (t, 1H, Ind-H), 7.25 (m, 2H, Ind-H), 7.61 (m, 2H, Ind-H).

1. customevaporated in vacuo
2. customleaving light yellow solid
3. extractionThe solid was extracted with dichloromethane (100 mL
4. filtration3×10 mL) and the extracts were filtered
5. customto give beige solid
6. customThe solution was evaporated in vacuo
7. customleaving fluffy yellow solid
8. washThe solid was washed with pentane (2×20 mL)
9. customdried in vacuo