Toluene → HCID 178420721, Verbindung

HRID 1198314Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1198314
[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

Komponenten

7

Reaktionsbedingungen

Temperatur
-20 °C

Versuchsvorschrift

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.

Aufarbeitung

  1. customThe mixture thus obtained
  2. customto reach room temperature
  3. additionwas slowly added
  4. customthe solvents were evaporated
  5. customThe solid material obtained
  6. customThe supernatant was decanted
  7. filtrationThe crystallized product was recovered by filtration

Quellen und Nachweise

ORD-Eintrag
ord-6a9d3bf2deec470c99d9fc1505ecd6f0
Quelldatensatz
uspto-grants-1994_01
Patentnummer
US05279999

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