HRID1072690

反应详情

EQUATION

反应方程式

HRID 1072690 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a yellow suspension of (pentamethylcyclopentadienyl)zirconium trichloride, Cp*ZrCl3, (5.00 g, 15.0 mmol, 1.00 equiv.) in ether (50 mL) was added lithium indenide (1.83 g, 15.0 mmol, 1.00 equiv.). The reaction turned slightly more manila-colored. The mixture was stirred 16 hours and then evaporated in vacuo, leaving yellow solid. The solid was extracted with dichloromethane (30 mL, then 3×5 mL) and the extracts were filtered to give light manila solid and a bright yellow solution. The solution was evaporated in vacuo, leaving yellow crystalline solid. The solid was washed with pentane (20 mL) and dried in vacuo. Yield 5.92 g (96%). 1H NMR(CD2Cl2): δ 2.03 (s, 15H, Me), 6.18 (d, 2H, Ind-H), 6.34 (t, 1H, Ind-H), 7.24 (m, 2H, Ind-H), 7.54 (m, 2H, Ind-H).

WORKUP

后处理

  1. customevaporated in vacuo
  2. customleaving yellow solid
  3. extractionThe solid was extracted with dichloromethane (30 mL
  4. filtration3×5 mL) and the extracts were filtered
  5. customto give light manila solid
  6. customThe solution was evaporated in vacuo
  7. customleaving yellow crystalline solid
  8. washThe solid was washed with pentane (20 mL)
  9. customdried in vacuo