HRID857845

反应详情

EQUATION

反应方程式

HRID 857845 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A suspension of 1.5 g (6.5 mmol) of lithium [1-(2-trimethylsiloxyethyl)indenide] in ether was added to a suspension of 2.2 g (6.5 mmol) of pentamethylcyclopentadienyl zirconium trichloride in 100 ml of ether at 0° C. After 30 minutes, the formation of a white solid was the volatiles were removed under vacuum to give a yellow oily-solid. This solid was recrystallized in hexane to give a mycrocristalline yellow solid, which was characterized as [1-(2-trimethylsiloxyethyl)indenyl]pentamethylcyclopentadienyl zirconium dichloride (1.7 g, 3.2 mmol, yield: 49%). 1H-NMR (CDCl3): 7.65 (m, 1H); 7.33 (m, 1H); 7.25 (m, 2H); 6.08 (m, 1H); 5.92 (m, 1H); 3.72 (dm, 2H); 3.28 (m, 1H); 2.72 (m, 1H); 2.04 (s, 15H); 0.03 (s, 9H). 13C-NMR (CDCl3): 131.4; 127.1; 126.7; 125.2; 125.1; 124.2; 123.5; 122.6; 116.1; 97.0; 62.6; 32.1; 12.5; −0.6.

WORKUP

后处理

  1. customwere removed under vacuum
  2. customto give a yellow oily-solid
  3. customThis solid was recrystallized in hexane
  4. customto give a mycrocristalline yellow solid, which