Reacción #1148670

ord-14abfae50d6c461e89b34413a762b8c4

Ecuación de reacción

[Li][CH2]CCC
n-Butyl lithium
[Cl-].[Cl-].[Cl-].[Cl-].[Hf+4]
Hafnium tetrachloride
CC(C)(C)c1cc(C2=Cc3ccccc3C2)cc(C(C)(C)C)c1
2-(3,5-Di-t-butylphenyl)indene
CC(C)(C)c1cc(C2=Cc3ccccc3[CH]2[Hf+2][CH]2C(c3cc(C(C)(C)C)cc(C(C)(C)C)c3)=Cc3ccccc32)cc(C(C)(C)C)c1.[Cl-].[Cl-]
product
Rendimiento 72.0%
CC(C)(C)c1cc(C2=Cc3ccccc3[CH]2[Hf+2][CH]2C(c3cc(C(C)(C)C)cc(C(C)(C)C)c3)=Cc3ccccc32)cc(C(C)(C)C)c1.[Cl-].[Cl-]
Bis(2-(3,5-di-t-butylphenyl)indenyl)hafnium dichloride
Rendimiento 72.0%

Condiciones de reacción

Temperatura
-10°CELSIUS
Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    workup.STIRRINGThe mixture was then stirred overnight
  2. 2
    Filtraciónthe solids were collected by filtration
  3. 3
    Otrothe residual solids were removed by filtration through celite
  4. 4
    LavadoThe celite was washed with an additional 100 mL of dichloromethane
  5. 5
    Otrothe solvents were evaporated

Procedimiento

2-(3,5-Di-t-butylphenyl)indene (23.3 g, 0.077 mol), and anhydrous diethyl ether (250 mL) were placed in a 1 L three-necked flask under argon. n-Butyl lithium (48 mL of a 1.6 M solution in hexanes, 0.077 mol) was added over a thirty minute period at 0° C. The solution was stirred for an additional two hours. Hafnium tetrachloride (12.2 g, 0.038 mol), was added incrementally over a one hour period. The mixture was then stirred overnight. The ethereal solution was chilled to −10° C. and the solids were collected by filtration. The solids were taken up in 300 mL of dichloromethane and the residual solids were removed by filtration through celite. The celite was washed with an additional 100 mL of dichloromethane, and the solvents were evaporated to give 23.5 g of product (72%).

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US06960550B2uspto-grants-2005_11