Toluene → HCID 178455874, compound
Reaction equation
CN([Zr:4](N(C)C)(N(C)C)N(C)C)C.C([CH:17]1[C:25]2[C:20](=[CH:21][CH:22]=[CH:23][CH:24]=2)[CH:19]=[CH:18]1)C=C.[Si]([Cl:30])(C)(C)C.[C:31]1([CH3:37])C=CC=C[CH:32]=1>>[Cl-:30].[Cl-:30].[Cl-:30].[CH2:37]([Zr+3:4][CH:17]1[C:25]2[C:20](=[CH:21][CH:22]=[CH:23][CH:24]=2)[CH:19]=[CH:18]1)[CH:31]=[CH2:32]Participants
Procedure
To Tetrakis(dimethylamino)zirconium (0.52 g, 1.94 mmol) dissolved in toluene (6 mL) was added allylindene (0.31 g, 1.99 mmol) at room temperature. The mixture was stirred at room temperature overnight. To the mixture was added Me3SiCl (1 mL, 7.9 mmol) at room temperature. The mixture was stirred at room temperature overnight. Removal of the solvent gave a yellow solid (crude allylindenylzirconium trichloride). The yellow solid (crude allylindenylzirconium trichloride) was dissolved in THF (10 mL). N-BuCpLi (0.276 g, 2.15 mmol) dissolved in THF (6 mL) was added to above THF solution (allylindenylzirconium trichloride/THF solution) at 0° C. The mixture was stirred at 0° C. for 30 minutes, then warned to room temperature and stirred for another 2.5 hours. The solvent was removed. The residue was extracted with toluene (30 mL). The supernatant was separated from the solid. Removal of the solvent gave a yellow solid. The yellow solid was washed with pentane (30 mL) and then dried under vacuum. The desired compound was obtained as a pale yellow solid (0.54 g, 64% overall yield). The product was identified by 1H-NMR (FIG. 2).
Workup
- stirringThe mixture was stirred at room temperature overnight
- customRemoval of the solvent
Sources & evidence
- ORD record
- ord-20670803e3fc462088f4c2682ee21e02
- Source dataset
- uspto-grants-2011_09
- Patent number
- US08013177B2
Reaction notes
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