반응 #498997

반응 방정식

n-Butyllithium

Zirconium tetrachloride

2-(3,5-Di-t-butylphenyl)indene

→

product

수율 64.0%

Bis(2-(3,5-di-t-Butylphenyl)indenyl)zirconium Dichloride

수율 64.0%

용매

—

hexanes

diethyl ether

반응 조건

후처리

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

실험 절차

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) was 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%).

출처