Toluene → Titanocene dichioride

HRID 865319Notes

Reaction equation

HRID 865319 reaction equation
[Li][Li].[Cl-:3].[Ti+4:4].[Cl-].[Cl-].[Cl-].[C:8]1([CH3:14])[CH:13]=[CH:12][CH:11]=CC=1>>[Cl-:3].[Cl-:3].[CH-:11]1[CH:12]=[CH:13][CH:8]=[CH:14]1.[CH-:11]1[CH:12]=[CH:13][CH:8]=[CH:14]1.[Ti+2:4]

Participants

4

Reactant 3

HCID 1140TolueneHCID 139759Lithium, mol. (Li2)HCID 160960Diamminetetrachlorotitanate(IV)

Product 1

HCID 124040768Titanocene dichiorideYield 13%

Conditions

Temperature
-78 °C

Procedure

A suspension of 5.46 g (17.5 mmol) of the dilithium etherate (Example 2) in 200 ml of toluene is cooled to -78° C., and 3.3 g (17.5 mmol) of titanium chloride are added. The reaction solution immediately becomes a dark red color. The mixture is stirred at room temperature for 30 hours, insoluble constituents are removed by filtration through a frit, and the dark-red toluene phase is evaporated to dryness in an oil-pump vacuum. Repeated washing with pentane gives 1.85 g of the titanocene dichioride as a brown-beige powder. The crude product is subsequently extracted for several days with pentane in a circulation frit, giving, after removal of the solvent, the titanocene dichloride as a brown solid in a yield of 13% (780 mg): m.p. 259° C. (decomp.,DSC).

Workup

  1. custominsoluble constituents are removed by filtration through a frit
  2. customthe dark-red toluene phase is evaporated to dryness in an oil-pump vacuum
  3. washRepeated washing with pentane

Sources & evidence

ORD record
ord-1820d463eb7845caa4e851ff6da50dd9
Source dataset
uspto-grants-1996_10
Patent number
US05565534

Reaction notes

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