反応 #1148670

反応方程式

n-Butyl lithium

Hafnium tetrachloride

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

→

product

収率 72.0%

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

収率 72.0%

溶媒

—

hexanes

diethyl ether

反応条件

後処理

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

実験手順

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%).

出典