Nitrogen → 6-(10-Naphthalen-2-ylanthracen-9-yl)phenanthrene

HRID 879921

Reaktionsgleichung

Reaktionsgleichung von HRID 879921
[CH:1]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH:4]=[CH:3][C:2]=1[C:11]1[C:24]2[C:19](=[CH:20][CH:21]=[CH:22][CH:23]=2)[C:18]([C:25]2[CH:26]=[C:27]3[C:36](=[CH:37][CH:38]=2)[C:35](C(O)=O)=[CH:34][C:33]2[CH:32]=[CH:31][CH:30]=[CH:29][C:28]3=2)=[C:17]2[C:12]=1[CH:13]=[CH:14][CH:15]=[CH:16]2.N#N.CO.O>N1C2C(=CC=CC=2)C=CC=1.[Cr]([O-])([O-])=O.[Cu+2]>[CH:1]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH:4]=[CH:3][C:2]=1[C:11]1[C:12]2[C:17](=[CH:16][CH:15]=[CH:14][CH:13]=2)[C:18]([C:25]2[CH:26]=[C:27]3[C:36](=[CH:37][CH:38]=2)[CH:35]=[CH:34][C:33]2[CH:32]=[CH:31][CH:30]=[CH:29][C:28]3=2)=[C:19]2[C:24]=1[CH:23]=[CH:22][CH:21]=[CH:20]2

Komponenten

6

Edukt 3

HCID 947NitrogenHCID 22242641Methanol--water (1/1)HCID 596294876-(10-Naphth-2-ylanthracen-9-yl)phenanthrene-9-carboxylic acid

Produkt 1

HCID 581944306-(10-Naphthalen-2-ylanthracen-9-yl)phenanthrene

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 178505374HCID 178505374, VerbindungKatalysatorHCID 7047QuinolineLösungsmittel

Versuchsvorschrift

49 g (94 mmol) of 6-(10-naphth-2-ylanthracen-9-yl)phenanthrene-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 8 h. 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 four times from chlorobenzene and sublimed twice in vacuo (p=1×10−5 mbar, T=360° C.). The yield is 32 g (71%) with a purity>99.9%.

Aufarbeitung

  1. additionare added
  2. temperaturethe mixture is heated at the boil for 8 h
  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 four times from chlorobenzene
  9. customsublimed twice in vacuo (p=1×10−5 mbar, T=360° C.)

Quellen und Nachweise

ORD-Eintrag
ord-aad495be30e24421a7bc140a5134821f
Quelldatensatz
uspto-grants-2015_03
Patentnummer
US08993123B2

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