Potassium hydride → HCID 178478635, Verbindung

HRID 2304942Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2304942
[H-].[K+].[N:3]1[C:12]2[C:7](=[CH:8][CH:9]=[CH:10][C:11]=2[CH:13]2[C:21]3[C:16](=[CH:17][CH:18]=[CH:19][CH:20]=3)[CH:15]=[CH:14]2)[CH:6]=[CH:5][CH:4]=1.[Cl-:22].[Cr+3:23].[Cl-].[Cl-]>C1COCC1>[Cl-:22].[Cl-:22].[N:3]1[C:12]2[C:7](=[CH:8][CH:9]=[CH:10][C:11]=2[CH:13]2[C:21]3[C:16](=[CH:17][CH:18]=[CH:19][CH:20]=3)[CH:15]=[C:14]2[Cr+2:23])[CH:6]=[CH:5][CH:4]=1

Komponenten

5

Edukt 3

HCID 82127Potassium hydrideHCID 6452300Chromium(3+) trichlorideHCID 219779971-(8-Quinolyl)indene

Produkt 1

HCID 178478635HCID 178478635, VerbindungAusbeute 50 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel2×

Versuchsvorschrift

0.05 g of potassium hydride (1.23 mmol) was suspended in 20 ml of THF, and 0.3 g of 1-(8-quinolyl)indene (1.23 mmol) was slowly added. The resultant violet suspension was stirred at room temperature for three hours and then added dropwise to a mixture of 0.46 g of chromium(III) chloride 3THF (1.23 mmol) in 50 ml of THF and, when the addition was complete, the mixture was stirred for a further 16 hours. The solvent was removed under reduced pressure, and the resultant solid was extracted with hot toluene. After the solvent had been distilled off from the combined extracts, the product was obtained as a green powder, which was washed a number of times with hexane and dried under a high vacuum, giving 0.22 g of 1-(8-quinolyl)indenylchromium(III) dichloride (50%).

Aufarbeitung

  1. additionwhen the addition
  2. stirringthe mixture was stirred for a further 16 hours
  3. customThe solvent was removed under reduced pressure
  4. extractionthe resultant solid was extracted with hot toluene
  5. distillationAfter the solvent had been distilled off from the combined extracts
  6. customthe product was obtained as a green powder, which
  7. washwas washed a number of times with hexane
  8. customdried under a high vacuum

Quellen und Nachweise

ORD-Eintrag
ord-7d59ab0c2c5f46aeb24fdc081cb54976
Quelldatensatz
uspto-grants-2002_08
Patentnummer
US06437161B1

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