Hafnium chloride (HfCl4) (6CI,8CI); Hafnium chloride; Hafnium tetrachloride; Hafnium(IV) chloride; Hafnium chloride (HfCl4), (T-4)- → HCID 178504164, compound

HRID 1017166Notes

Reaction equation

HRID 1017166 reaction equation
[CH3:1][Si:2]([CH3:23])([CH3:22])[C:3]1[CH:4]=[C:5]([C:13]2[CH2:14][C:15]3[C:20]([CH:21]=2)=[CH:19][CH:18]=[CH:17][CH:16]=3)[CH:6]=[C:7]([Si:9]([CH3:12])([CH3:11])[CH3:10])[CH:8]=1.[CH2:24]([Li])[CH2:25][CH2:26][CH3:27].[Cl-:29].[Cl-].[Cl-].[Cl-].[Hf+4:33]>C(OCC)C>[Cl-:29].[Cl-:29].[CH3:12][Si:9]([CH3:10])([CH3:11])[C:7]1[CH:6]=[C:5]([C:13]2[CH:14]([Hf+2:33][CH:24]3[C:15]4[C:27](=[CH:20][CH:21]=[CH:13][CH:14]=4)[CH:26]=[C:25]3[C:5]3[CH:6]=[C:7]([Si:9]([CH3:10])([CH3:12])[CH3:11])[CH:8]=[C:3]([Si:2]([CH3:23])([CH3:1])[CH3:22])[CH:4]=3)[C:15]3[C:20]([CH:21]=2)=[CH:19][CH:18]=[CH:17][CH:16]=3)[CH:4]=[C:3]([Si:2]([CH3:23])([CH3:22])[CH3:1])[CH:8]=1

Participants

5

Reactant 3

HCID 9927068Hafnium chloride (HfCl4) (6CI,8CI); Hafnium chloride; Hafnium tetrachloride; Hafnium(IV) chloride; Hafnium chloride (HfCl4), (T-4)-HCID 222838172-(3,5-Bis(trimethylsilyl)phenyl)indeneHCID 178418339Butyllithium

Product 1

HCID 178504164HCID 178504164, compoundYield 56%

Reagents, catalysts & solvents 1

HCID 3283Diethyl EtherSolvent

Conditions

Temperature
-10 °C

Procedure

2-(3,5-Bis(trimethylsilyl)phenyl)indene (22.3 g, 0.066 mol) and anhydrous diethyl ether (250 mL) were placed in a 1 L three-necked flask under argon. n-Butyllithium (41 mL of a 1.6 M solution in hexanes, 0.066 mol) was added over a thirty minute period at 0° C. The solution was stirred for an additional two hours. Hafnium tetrachloride (10.5 g, 0.033 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 17.3 g of bis(2-(3,5-bis(trimethylsilyl)phenyl)indenyl)hafnium dichloride product (56% yield).

Workup

  1. stirringThe mixture was then stirred overnight
  2. filtrationthe solids were collected by filtration
  3. customthe residual solids were removed by filtration through celite
  4. washThe celite was washed with an additional 100 mL of dichloromethane
  5. customthe solvents were evaporated

Sources & evidence

ORD record
ord-b3afda65ad6345498d1d88a4b6051006
Source dataset
uspto-grants-2002_11
Patent number
US06479424B1

Reaction notes

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