Reacción #1148669

ord-d064166f6363433d86de9fba26f62887

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
    Otrothe solids were collected
  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 (13.8 g, 0.045 mol) and anhydrous diethyl ether (250 mL) were placed in a 1 L three-necked flask under argon. n-Butyllithium (28 mL of a 1.6 M solution in hexanes, 0.045 mol) as added over a thirty minute period at 0° C. The solution was stirred for an additional two hours. Zirconium tetrachloride (5.1 g, 0.022 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. 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 11.2 g of product (64%).

Fuente

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