반응 #1148670

반응 방정식

n-Butyl lithium

Hafnium tetrachloride

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

→

product

수율 72.0%

Bis(2-(3,5-di-t-butylphenyl)indenyl)hafnium dichloride

수율 72.0%

용매

—

hexanes

diethyl ether

반응 조건

후처리

1. 1
   workup.STIRRINGThe mixture was then stirred overnight
2. 2
   여과the solids were collected by filtration
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 (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%).

출처