HCID 178418348, compound → HCID 178420594, compound

HRID 1032894Notes

Reaction equation

HRID 1032894 reaction equation
[Cl-].[Cl-].[CH:3]1([Zr+2:8][CH:9]2[CH:13]=[CH:12][CH:11]=[CH:10]2)[CH:7]=[CH:6][CH:5]=[CH:4]1.C[Li]>CCCCCC>[CH:9]1([Zr:8][CH:3]2[CH:7]=[CH:6][CH:5]=[CH:4]2)[CH:10]=[CH:11][CH:12]=[CH:13]1

Participants

4

Reactant 2

HCID 178418348HCID 178418348, compoundHCID 178420591HCID 178420591, compound

Product 1

HCID 178420594HCID 178420594, compound

Reagents, catalysts & solvents 1

HCID 8058HexaneSolvent

Conditions

Temperature
0 °C

Procedure

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.

Workup

  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

Sources & evidence

ORD record
ord-a822b72b5ddc4792b801ed1fd4da0677
Source dataset
uspto-grants-1994_05
Patent number
US05308811

Reaction notes

Loading…