تفاعل #1148669

ord-d064166f6363433d86de9fba26f62887

معادلة التفاعل

[Li][CH2]CCC
n-Butyllithium
[Cl-].[Cl-].[Cl-].[Cl-].[Zr+4]
Zirconium 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[Zr+2][CH]2C(c3cc(C(C)(C)C)cc(C(C)(C)C)c3)=Cc3ccccc32)cc(C(C)(C)C)c1.[Cl-].[Cl-]
product
المردود 64.0%
CC(C)(C)c1cc(C2=Cc3ccccc3[CH]2[Zr+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)zirconium dichloride
المردود 64.0%

المذيبات

ظروف التفاعل

درجة الحرارة
-10°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

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

الإجراء التجريبي

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%).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US06960550B2uspto-grants-2005_11