Lithium, 1H-inden-1-yl- → HCID 178426005, compound

HRID 1072690Notes

Reaction equation

HRID 1072690 reaction equation
[Cl-:1].[Cl-].[Cl-].[CH3:4][C:5]1[C:9]([Zr+3:11])([CH3:10])[C:8]([CH3:12])=[C:7]([CH3:13])[C:6]=1[CH3:14].[CH-:15]1[C:23]2[C:18](=[CH:19][CH:20]=[CH:21][CH:22]=2)[CH:17]=[CH:16]1.[Li+]>CCOCC>[Cl-:1].[Cl-:1].[CH3:4][C:5]1[C:9]([Zr+2:11][CH:15]2[C:23]3[C:18](=[CH:19][CH:20]=[CH:21][CH:22]=3)[CH:17]=[CH:16]2)([CH3:10])[C:8]([CH3:12])=[C:7]([CH3:13])[C:6]=1[CH3:14]

Participants

4

Reactant 2

HCID 11116044Lithium, 1H-inden-1-yl-HCID 178426006HCID 178426006, compound

Product 1

HCID 178426005HCID 178426005, compound

Reagents, catalysts & solvents 1

HCID 3283Diethyl EtherSolvent

Procedure

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

  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

Sources & evidence

ORD record
ord-582f89ae26d2456e818a9c7a8f3d508c
Source dataset
uspto-grants-2005_06
Patent number
US06911508B2

Reaction notes

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