2,4-Dimethylphenol → HCID 178421919, compound

HRID 1827257Notes

Reaction equation

[CH3:1][C:2]1[CH:7]=[C:6]([CH3:8])[CH:5]=[CH:4][C:3]=1[OH:9].C1COCC1.C([Li])CCC.[Cl-:20].[Cl-].[CH3:22][Zr:23]([CH3:45])(=[SiH2:44])([CH:34]1[C:42]2[C:37](=[CH:38][CH:39]=[CH:40][CH:41]=2)[CH:36]=[C:35]1[CH3:43])[CH:24]1[C:32]2[C:27](=[CH:28][CH:29]=[CH:30][CH:31]=2)[CH:26]=[C:25]1[CH3:33]>C1(C)C=CC=CC=1>[CH3:1][C:2]1[CH:7]=[C:6]([CH3:8])[CH:5]=[CH:4][C:3]=1[O-:9].[Cl-:20].[CH3:45][Zr:23]([CH3:22])(=[SiH2:44])([CH:34]1[C:42]2[C:37](=[CH:38][CH:39]=[CH:40][CH:41]=2)[CH:36]=[C:35]1[CH3:43])[CH:24]1[C:32]2[C:27](=[CH:28][CH:29]=[CH:30][CH:31]=2)[CH:26]=[C:25]1[CH3:33]

Participants

Conditions

Temperature: 60 °C

Procedure

1.0 g (8.2 mmol) of 2,4-dimethylphenol in 20 ml of toluene/2 ml of THF was admixed at room temperature with 3.0 ml (8.2 mmol) of a 20% strength solution of butyllithium in toluene. The mixture was stirred for another 1 hour at 60° C. At room temperature, 1.9 g (4.0 mmol) of dimethylsilanediylbis(2-methylindenyl)zirconium dichloride were added as a solid. The suspension was stirred for 8 hours at 60° C. and subsequently filtered hot through Celite. After evaporation of the solvent to leave a volume of about 7 ml, the yellow solid which precipitated at −30° C. was filtered off and dried under reduced pressure. This gave 0.65 g (29%) of dimethylsilanediylbis(2-methylindenyl)zirconium monochloride mono(2,4-di-methylphenoxide) (5).

Workup

stirringThe suspension was stirred for 8 hours at 60° C. and subsequently filtered hot through Celite
customAfter evaporation of the solvent
customto leave a volume of about 7 ml
customthe yellow solid which precipitated at −30° C.
filtrationwas filtered off
customdried under reduced pressure

Sources & evidence

ORD record: ord-da77f0a1e7144e0cbc38463cc0f4b64d
Source dataset: uspto-grants-2006_05
DOI: 10.6084/m9.figshare.5104873.v1
Patent number: US07053160B1

Reaction notes

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