Toluene → HCID 178477763, compound

HRID 1681443Notes

Reaction equation

HRID 1681443 reaction equation
Cl[C:2](=[Ti:4]([CH:10]1[CH:14]=[CH:13][CH:12]=[CH:11]1)[CH:5]1[CH:9]=[CH:8][CH:7]=[CH:6]1)Cl.C1(C)C=CC=CC=1.[CH3:22][Al:23]1[CH2:28][CH2:27][CH2:26][CH2:25][O:24]1.CCCCCC>C1C=CC=CC=1>[CH2:2]=[Ti:4]([CH:5]1[CH:6]=[CH:7][CH:8]=[CH:9]1)[CH:10]1[CH:14]=[CH:13][CH:12]=[CH:11]1.[CH3:22][Al:23]1[CH2:28][CH2:27][CH2:26][CH2:25][O:24]1

Participants

6

Reactant 4

HCID 1140TolueneHCID 8058HexaneHCID 23511181MethylalumoxaneHCID 178478494HCID 178478494, compound

Product 1

HCID 178477763HCID 178477763, compoundYield 82%

Reagents, catalysts & solvents 1

HCID 241BenzeneSolvent

Conditions

Temperature
-20 °C

Procedure

In a nitrogen-purged Schlenk reaction vessel, 97.4 mg (0.37 mmol) of dichloromethylenebis(cyclopentadienyl)titanium was weighted out. Thereto 20 ml of dried toluene was added, and the mixture was cooled to -20° C. A solution of 1.4 mmol of methylalumoxane (tetramer) in benzene was added thereto dropwise with stirring over one hour. The reaction solution was gradually brought to room temperature, and then stirred continuously for 2 days. The reaction solution changed gradually its color from violet to reddish brown. Hexane was added thereto, and the formed precipitate was collected by filtration, dried and recrystallized. The yield was 82%.

Workup

  1. customIn a nitrogen-purged Schlenk reaction vessel
  2. customwas gradually brought to room temperature
  3. stirringstirred continuously for 2 days
  4. filtrationthe formed precipitate was collected by filtration
  5. customdried
  6. customrecrystallized

Sources & evidence

ORD record
ord-20f1cf1f102d436490a6f219f35078e1
Source dataset
uspto-grants-1992_12
Patent number
US05171871

Reaction notes

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