Lithium [1-(2-trimethylsiloxyethyl)indenide] → HCID 178504312, compound

HRID 857845Notes

Reaction equation

HRID 857845 reaction equation
[CH3:1][Si:2]([CH3:16])([CH3:15])[O:3][CH2:4][CH2:5][C-:6]1[C:14]2[C:9](=[CH:10][CH:11]=[CH:12][CH:13]=2)[CH:8]=[CH:7]1.[Li+].[Cl-:18].[Cl-].[Cl-].[CH3:21][Zr:22]([CH3:31])([CH3:30])([CH3:29])([CH3:28])[CH:23]1[CH:27]=[CH:26][CH:25]=[CH:24]1>CCOCC>[Cl-:18].[Cl-:18].[CH3:16][Si:2]([CH3:15])([CH3:1])[O:3][CH2:4][CH2:5][CH:6]1[C:14]2[C:9](=[CH:10][CH:11]=[CH:12][CH:13]=2)[CH:8]=[C:7]1[Zr:22]([CH3:31])([CH3:30])([CH3:29])([CH3:28])([CH3:21])[CH:23]1[CH:27]=[CH:26][CH:25]=[CH:24]1

Participants

4

Reactant 2

HCID 86589894Lithium [1-(2-trimethylsiloxyethyl)indenide]HCID 178477801HCID 178477801, compound

Product 1

HCID 178504312HCID 178504312, compoundYield 98.5%

Reagents, catalysts & solvents 1

HCID 3283Diethyl EtherSolvent2×

Procedure

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

  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

Sources & evidence

ORD record
ord-49817c43889943948ba197883a2d2082
Source dataset
uspto-grants-2006_12
Patent number
US07148173B2

Reaction notes

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