HCID 178461830, compound → HCID 178461830, compound

HRID 1078082Notes

Reaction equation

[Cl-:1].[Cl-].[CH:3]([Zr+2:6]([CH:12]1[C:24]2[CH:23]=[CH:22][CH:21]=[CH:20][C:19]=2[C:18]2[C:13]1=[CH:14][CH:15]=[CH:16][CH:17]=2)[CH:7]1[CH:11]=[CH:10][CH:9]=[CH:8]1)([CH3:5])[CH3:4]>C1(C)C=CC=CC=1>[Zr:6].[Cl-:1].[Cl-:1].[CH:3]([Zr+2:6]([CH:12]1[C:24]2[CH:23]=[CH:22][CH:21]=[CH:20][C:19]=2[C:18]2[C:13]1=[CH:14][CH:15]=[CH:16][CH:17]=2)[CH:7]1[CH:11]=[CH:10][CH:9]=[CH:8]1)([CH3:5])[CH3:4]

Participants

Conditions

Temperature: 80 °C

Procedure

At the same time, 65 mg (0.15 mmol) of isopropyl-(9-fluorenyl)cyclopentadienylzirconium dichloride are dissolved in 40 ml of toluene and added dropwise to the suspension. The cold reaction mixture is introduced into a microwave apparatus. While stirring in an inert gas stream at a microwave frequency of 2.45 GHz and microwave power of 500 W, the mixture is heated to 80° C. over a period of 15 minutes, the suspension taking on a red color. The radiation power is adjusted so that the suspension is maintained at this temperature for one hour (250 W, pulsed). The mixture is subsequently filtered and the red dye is washed three times with 50 ml of toluene. Analysis of the pale red filtrate gives a zirconium content of 0.9 mg (corresponds to 4.3 mg of isopropyl-(9-fluorenyl)cyclopentadienylzirconium dichloride). The solid is dried in vacuo. 3 g of free-flowing violet supported catalyst containing 20 mg of zirconocene per gram of catalyst are obtained.

Workup

additionadded dropwise to the suspension
customThe cold reaction mixture
additionis introduced into a microwave apparatus
temperatureis maintained at this temperature for one hour (250 W, pulsed)
filtrationThe mixture is subsequently filtered
washthe red dye is washed three times with 50 ml of toluene

Sources & evidence

ORD record: ord-a54230ff888d42388ddf3dfdac0e5aeb
Source dataset: uspto-grants-1996_08
DOI: 10.6084/m9.figshare.5104873.v1
Patent number: US05545829

Reaction notes

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