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Zirconium chloride (ZrCl4), (T-4)- → Zirconium(2+) dicyclopenta-2,4-dien-1-ide

HRID 52679
ノート
印刷プレビュー

反応式

HRID 52679 の反応式
[CH:1]1(C(C2C3C=CC=CC=3C3C2=CC=CC=3)(C)CCC=C)[CH:5]=[CH:4][CH:3]=[CH:2]1.[Cl-].[Cl-].[Cl-].[Cl-].[Zr+4:29]>Cl[SiH](C)C.[H+].[H+].Cl[Pt-2](Cl)(Cl)(Cl)(Cl)Cl>[CH-:1]1[CH:5]=[CH:4][CH:3]=[CH:2]1.[CH-:1]1[CH:5]=[CH:4][CH:3]=[CH:2]1.[Zr+2:29]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 9856075Zirconium chloride (ZrCl4), (T-4)-HCID 158619165-Cyclopentadienyl-5-(9-fluorenyl)-1-hexene

生成物 1

HCID 15183825Zirconium(2+) dicyclopenta-2,4-dien-1-ide

試薬・触媒・溶媒 2

HCID 61859Chloroplatinic acid触媒HCID 66108Chlorodimethylsilane溶媒

実験手順

Then 1.61 g of the bridged ligand having a vinyl terminated branch, i.e. 5-cyclopentadienyl-5-(9-fluorenyl)-1-hexene, was dissolved in 10 mL of chlorodimethylsilane at room temperature. Then approximately 1 mL of hexachloroplatinic acid was added and a reaction mixture stirred overnight at room temperature. The solvent was then evaporated in a vacuum. A white solid was recovered which was concluded to be 1-chlorodimethyl-silyl-5-cyclopentadienyl-5-(9-fluorenyl)-hexane. A portion of this material was then contacted with silica gel (Merck No. 7734) the process involved contacting 2 g of the silica gel dried as explained in Example IV and 1.56 g of the 1-chlorodimethyl-silyl-5-cyclopentadienyl-5-(9-fluorenyl)-hexane in a manner analogous to that used in the analogous step in Example IV. Then a supported zirconocene was prepared by reacting 1.74 g of that solid with 0.8 g of zirconium tetrachloride using a technique of the general type disclosed in Example IV. The resulting supported metallocene will be referred to herein as catalyst 34A.

後処理

  1. customThe solvent was then evaporated in a vacuum
  2. customA white solid was recovered which
  3. customdried

出典と根拠

ORDレコード
ord-7462102bc6c743e9b4de7098568f19de
出典データセット
uspto-grants-1997_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05616752

反応ノート

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