Toluene → HCID 178461101, compound

HRID 1280335Notes

Reaction equation

CC([CH:9]1[C:24]2[C:23]3[CH:22]=[CH:21][CH:20]=[CH:19][C:18]=3[N:17]([C:25]3[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=3)[C:16]=2[C:15]2[C:10]1=[CH:11][CH:12]=[CH:13][CH:14]=2)(C1C=CC=C1)C.[C:31]1([CH3:37])[CH:36]=[CH:35][CH:34]=CC=1.[Li][CH2:39][CH2:40][CH2:41]C.[Cl-:43].[Cl-].[Cl-].[Cl-].[Zr+4:47]>CCCCCC>[Cl-:43].[Cl-:43].[C:40](=[Zr+2:47]([CH:9]1[C:24]2[C:23]3[CH:22]=[CH:21][CH:20]=[CH:19][C:18]=3[N:17]([C:25]3[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=3)[C:16]=2[C:15]2[C:10]1=[CH:11][CH:12]=[CH:13][CH:14]=2)[CH:37]1[CH:31]=[CH:36][CH:35]=[CH:34]1)([CH3:41])[CH3:39]

Participants

Conditions

Temperature: -50 °C

Procedure

In a 70 ml bulb were placed 2.26 g (6 mmol) of the ligand 10-[1-methyl-1-(cyclopentadienyl)ethyl]N-phenyl-5,10-dihydroindeno[1,2-b]indole, prepared in Example 16, and 20 ml of toluene. The obtained mixture was cooled to −50° C. and treated with 7.5 ml (12 mmol) of BuLi 1.6N in hexane. The resulting solution was allowed to warm to room temperature within 1 hour and then it was treated with 1.4 g (6 mmol) of ZrCl4. The solvent was evaporated and the residue was recrystallized from ether, thus yielding 0.55 g of isopropyliden(N-phenyl-5,10-dihydroindeno[1,2-b]indol-10-yl)(cyclopentadienyl) zirconium dichloride (yield=17%).

Workup

temperatureto warm to room temperature within 1 hour
customThe solvent was evaporated
customthe residue was recrystallized from ether

Sources & evidence

ORD record: ord-bdee2053dae74cd99b03ab2f1c89a08a
Source dataset: uspto-grants-2002_09
DOI: 10.6084/m9.figshare.5104873.v1
Patent number: US06451724B1

Reaction notes

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