Toluene → HCID 178420721, compound

HRID 1198314Notes

Reaction equation

[CH2:1]([Li])[CH2:2][CH2:3][CH3:4].[CH3:6][CH2:7][CH2:8][CH2:9][CH2:10][CH3:11].[C:12]1([C:18]2[CH2:22][CH:21]=[C:20]([C:23]3[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=3)[CH:19]=2)[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1.[Cl-:29].[Cl-].[Cl-].[Cl-].[Zr+4:33].[C:34]1([CH3:40])[CH:39]=[CH:38][CH:37]=[CH:36][CH:35]=1>O1CCCC1>[Cl-:29].[Cl-:29].[C:8]1([C:2]2([Zr+2:33][C:20]3([C:23]4[CH:24]=[CH:25][CH:26]=[CH:27][CH:28]=4)[CH:21]=[CH:22][C:18]([C:12]4[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=4)=[CH:19]3)[CH:3]=[CH:4][C:40]([C:34]3[CH:39]=[CH:38][CH:37]=[CH:36][CH:35]=3)=[CH:1]2)[CH:7]=[CH:6][CH:11]=[CH:10][CH:9]=1

Participants

Conditions

Temperature: -20 °C

Procedure

A solution (1.4 ml) of n-butyllithium in hexane (1.6 mole/liter, 0.0023 mole n-butyllithium) at 80° C. was added slowly to 0.50 g (0.0023 mole) of 1,3-diphenylcyclopentadiene dissolved in 20 ml tetrahydrofuran. The mixture thus obtained was allowed to reach room temperature. A mixture of 0.268 g (0.00115 mole) of zirconium tetrachloride in 10 ml tetrahydrofuran was slowly added. After stirring the mixture for two hours, the solvents were evaporated. The solid material obtained was taken up in toluene and centrifuged. The supernatant was decanted and cooled to -20° C. The crystallized product was recovered by filtration.

Workup

customThe mixture thus obtained
customto reach room temperature
additionwas slowly added
customthe solvents were evaporated
customThe solid material obtained
customThe supernatant was decanted
filtrationThe crystallized product was recovered by filtration

Sources & evidence

ORD record: ord-6a9d3bf2deec470c99d9fc1505ecd6f0
Source dataset: uspto-grants-1994_01
DOI: 10.6084/m9.figshare.5104873.v1
Patent number: US05279999

Reaction notes

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