Nitrogen → 9-Phenanthren-3-ylanthracene

HRID 879923

Reaktionsgleichung

Reaktionsgleichung von HRID 879923
[CH:1]1[C:14]2[C:5](=[CH:6][C:7]3[C:12]([C:13]=2[C:15]2[CH:16]=[C:17]4[C:26](=[CH:27][CH:28]=2)[C:25](C(O)=O)=[CH:24][C:23]2[CH:22]=[CH:21][CH:20]=[CH:19][C:18]4=2)=[CH:11][CH:10]=[CH:9][CH:8]=3)[CH:4]=[CH:3][CH:2]=1.N#N.CO.O>N1C2C(=CC=CC=2)C=CC=1.[Cr]([O-])([O-])=O.[Cu+2]>[CH:27]1[C:26]2[CH:25]=[CH:24][C:23]3[C:18](=[CH:19][CH:20]=[CH:21][CH:22]=3)[C:17]=2[CH:16]=[C:15]([C:13]2[C:12]3[C:7]([CH:6]=[C:5]4[C:14]=2[CH:1]=[CH:2][CH:3]=[CH:4]4)=[CH:8][CH:9]=[CH:10][CH:11]=3)[CH:28]=1

Komponenten

6

Edukt 3

HCID 947NitrogenHCID 22242641Methanol--water (1/1)HCID 596294916-Anthracen-9-ylphenanthrene-9-carboxylic acid

Produkt 1

HCID 596295009-Phenanthren-3-ylanthracene

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 178505374HCID 178505374, VerbindungKatalysatorHCID 7047QuinolineLösungsmittel

Versuchsvorschrift

40 g (94 mmol) of 6-anthracen-9-ylphenanthrene-9-carboxylic acid are suspended in 250 ml of quinoline, the suspension is saturated with N2, 11.8 g (38 mmol) of copper chromite are added, and the mixture is heated at the boil for eight hours. The mixture is subsequently poured into 1 l of MeOH/water, and the black solid is filtered off with suction, washed with MeOH and subjected to Soxhlet extraction with CHCl3. Removal of the solvent leaves a greyish solid, which is recrystallised twice from dioxane. The yield is 30.6 g (92%).

Aufarbeitung

  1. additionare added
  2. temperaturethe mixture is heated at the boil for eight hours
  3. filtrationthe black solid is filtered off with suction
  4. washwashed with MeOH
  5. extractionsubjected to Soxhlet extraction with CHCl3
  6. customRemoval of the solvent
  7. customleaves a greyish solid, which
  8. customis recrystallised twice from dioxane

Quellen und Nachweise

ORD-Eintrag
ord-fc400d9c518b466e9f83d4d1a64dc280
Quelldatensatz
uspto-grants-2015_03
Patentnummer
US08993123B2

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