Zirconium chloride (ZrCl4), (T-4)- → HCID 178440619, compound

HRID 1017165Notes

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-].[Zr+4:33]>C(OCC)C>[Cl-:29].[Cl-:29].[C:1]([C:5]1[CH:6]=[C:7]([C:15]2[CH:23]([Zr+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

Conditions

Temperature: -10 °C

Procedure

2-(3,5-Di-t-butylphenyl)indene (13.8 g, 0.045 mol) and anhydrous diethyl ether (250 mL) were placed in a 1 L three-necked flask under argon. n-Butyllithium (28 mL of a 1.6 M solution in hexanes, 0.045 mol) was added over a thirty minute period at 0° C. The solution was stirred for an additional two hours. Zirconium tetrachloride (5.1 g, 0.022 mol) was added incrementally over a one hour period. The mixture then was stirred overnight. The ethereal solution was chilled to −10° C. and the solids were collected. 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 11.2 g of product (64% yield).

Workup

stirringThe mixture then was stirred overnight
customthe solids were collected
customthe residual solids were removed by filtration through celite
washThe celite was washed with an additional 100 mL of dichloromethane
customthe solvents were evaporated

Sources & evidence

ORD record: ord-4d59c660d3434c4aa461772ec93c9f08
Source dataset: uspto-grants-2002_11
DOI: 10.6084/m9.figshare.5104873.v1
Patent number: US06479424B1

Reaction notes

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