Hafnium chloride (HfCl4) (6CI,8CI); Hafnium chloride; Hafnium tetrachloride; Hafnium(IV) chloride; Hafnium chloride (HfCl4), (T-4)- → HCID 178440618, compound

HRID 411816Notes

Reaction equation

HRID 411816 reaction equation
[C:1]([C:5]1[CH:6]=[C:7]([C:15]2[CH2:16][C:17]3[C:22]([CH:23]=2)=[CH:21][CH:20]=[CH:19][CH:18]=3)[CH:8]=[C:9]([C:11]([CH3:14])([CH3:13])[CH3:12])[CH:10]=1)([CH3:4])([CH3:3])[CH3:2].[CH2:24]([Li])[CH2:25][CH2:26][CH3:27].[Cl-:29].[Cl-].[Cl-].[Cl-].[Hf+4:33]>C(OCC)C>[Cl-:29].[Cl-:29].[C:1]([C:5]1[CH:6]=[C:7]([C:15]2[CH:23]([Hf+2:33][CH:24]3[C:17]4[C:27](=[CH:22][CH:23]=[CH:15][CH:16]=4)[CH:26]=[C:25]3[C:7]3[CH:6]=[C:5]([C:1]([CH3:3])([CH3:2])[CH3:4])[CH:10]=[C:9]([C:11]([CH3:14])([CH3:13])[CH3:12])[CH:8]=3)[C:22]3[C:17]([CH:16]=2)=[CH:18][CH:19]=[CH:20][CH:21]=3)[CH:8]=[C:9]([C:11]([CH3:14])([CH3:13])[CH3:12])[CH:10]=1)([CH3:2])([CH3:3])[CH3:4]

Participants

5

Reactant 3

HCID 9927068Hafnium chloride (HfCl4) (6CI,8CI); Hafnium chloride; Hafnium tetrachloride; Hafnium(IV) chloride; Hafnium chloride (HfCl4), (T-4)-HCID 222838282-(3,5-di-t-Butylphenyl)indeneHCID 178418339Butyllithium

Product 1

HCID 178440618HCID 178440618, compoundYield 72%

Reagents, catalysts & solvents 1

HCID 3283Diethyl EtherSolvent

Conditions

Temperature
-10 °C

Procedure

2-(3,5-Di-t-butylphenyl)indene (23.3 g, 0.077 mol), and anhydrous diethyl ether (250 mL) were placed in a 1 L three-necked flask under argon. n-Butyl lithium (48 mL of a 1.6 M solution in hexanes, 0.077 mol) was added over a thirty minute period at 0° C. The solution was stirred for an additional two hours. Hafnium tetrachloride (12.2 g, 0.038 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 23.5 g of product (72%).

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-aaac794e48c54e2aae09cf78413bc837
Source dataset
uspto-grants-2003_05
Patent number
US06559262B1

Reaction notes

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