Chromium(3+) trichloride → HCID 178425929, Verbindung

HRID 1005645

Reaktionsgleichung

Reaktionsgleichung von HRID 1005645
[CH3:1][C:2]1[CH:11]=[CH:10][C:9]2[C:4](=[C:5]([C:12]3[CH:16]([CH3:17])[C:15]([CH3:18])=[C:14]([CH3:19])[C:13]=3[CH3:20])[CH:6]=[CH:7][CH:8]=2)[N:3]=1.C([Li])CCC.[Cl-:26].[Cr+3:27].[Cl-].[Cl-]>C1COCC1>[Cl-:26].[Cl-:26].[CH3:1][C:2]1[CH:11]=[CH:10][C:9]2[C:4](=[C:5]([C:12]3([Cr+2:27])[C:16]([CH3:17])=[C:15]([CH3:18])[C:14]([CH3:19])=[C:13]3[CH3:20])[CH:6]=[CH:7][CH:8]=2)[N:3]=1

Komponenten

5

Edukt 3

HCID 6452300Chromium(3+) trichlorideHCID 223521291-(2-Methyl-8-quinolyl)-2,3,4,5-tetramethylcyclopentadieneHCID 178418339Butyllithium

Produkt 1

HCID 178425929HCID 178425929, VerbindungAusbeute 50 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel2×

Versuchsvorschrift

0.3 g of 1-(2-methyl-8-quinolyl)-2,3,4,5-tetramethylcyclopentadiene (1.14 mmol) in 30 ml of THF was deprotonated using 0.45 ml of n-butyllithium (2.5 M in hexane, 1.14 mmol). After the mixture had been stirred for two hours, the red solution was added dropwise to a suspension of chromium(III) chloride in 20 ml of THF. After the mixture had been stirred at room temperature for 16 hours, the solvents were evaporated off, and the resultant residue was taken up in 20 ml of toluene. The green suspension was filtered, and the residue was extracted a number of times with hot toluene. Conventional work-up gave the product as a green powder (0.22 g) in a yield of 50%.

Aufarbeitung

  1. stirringAfter the mixture had been stirred at room temperature for 16 hours
  2. customthe solvents were evaporated off
  3. filtrationThe green suspension was filtered
  4. extractionthe residue was extracted a number of times with hot toluene

Quellen und Nachweise

ORD-Eintrag
ord-26d5d53a78074334a7cbde7656159d3f
Quelldatensatz
uspto-grants-2004_09
Patentnummer
US06787498B2

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