反应详情

温度

0 °C

Into a 300 ml round bottom flask, 7.5 g of commercially available biscyclopentadienylzirconium dichloride was introduced, and the interior of the flask was thoroughly flushed with nitrogen. Then, 120 ml of ethyl ether was added thereto at -20° C. to obtain a slurry. To this slurry, 32 ml of a hexane solution of methyllithium (1.6M) was gradually added at -20° C, and the mixture was stirred at 0° C for 30 minutes. Then, the solvent was evaporated, and the remained solid was sublimed and purified under reduced pressure of 2×10-4 mmHg at a temperature of from 60 to 80° C to obtain biscyclopentadienylzirconium dimetyl. Separately, an aqueous solution containing 3.40 g of silver nitrate and 6.84 g of sodium tetraphenyl borate were mixed to obtain silver tetraphenyl borate.

1. customthe interior of the flask was thoroughly flushed with nitrogen
2. additionThen, 120 ml of ethyl ether was added
3. customat -20° C. to obtain a slurry
4. customThen, the solvent was evaporated
5. custompurified under reduced pressure of 2×10-4 mmHg at a temperature of from 60 to 80° C