1-Fluoronaphthalene → HCID 42640664, Verbindung

HRID 221180

Reaktionsgleichung

Reaktionsgleichung von HRID 221180
[Br:1][C:2]1[CH:3]=[CH:4][C:5]2[NH:6][C:7]3[C:12]([C:13]=2[CH:14]=1)=[CH:11][C:10]([Br:15])=[CH:9][CH:8]=3.F[C:17]1[C:26]2[C:21](=[CH:22][CH:23]=[CH:24][CH:25]=2)[CH:20]=[CH:19][CH:18]=1.C(=O)([O-])[O-].[Cs+].[Cs+]>CS(C)=O>[Br:15][C:10]1[CH:9]=[CH:8][C:7]2[N:6]([C:25]3[C:26]4[C:21](=[CH:20][CH:19]=[CH:18][CH:17]=4)[CH:22]=[CH:23][CH:24]=3)[C:5]3[C:13]([C:12]=2[CH:11]=1)=[CH:14][C:2]([Br:1])=[CH:3][CH:4]=3

Komponenten

5

Edukt 3

HCID 94501-FluoronaphthaleneHCID 10796Cesium carbonateHCID 2748743,6-Dibromocarbazole

Produkt 1

HCID 42640664HCID 42640664, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 679Dimethyl SulfoxideLösungsmittel

Reaktionsbedingungen

Temperatur
145 °C

Versuchsvorschrift

Into a flask, 10.00 g of 3,6-dibromo-9H-carbazole, 4.1 ml of 1-fluoronaphthalene, 12.06 g of cesium carbonate, and 300 ml of dimethylsulfoxide were put, and the solution was stirred at 145° C. for 36 hours under nitrogen atmosphere. After heating, the reaction liquid was cooled to room temperature and then filtrated, and the filtrates were concentrated by a vacuum pump. The concentrates were purified by silica gel column chromatography, and then washed by methanol, and thus 5.5 g of 3,6-dibromo-9-naphthalene-1-yl-carbazole was obtained.

Aufarbeitung

  1. temperatureAfter heating
  2. customthe reaction liquid
  3. temperaturewas cooled to room temperature
  4. filtrationfiltrated
  5. concentrationthe filtrates were concentrated by a vacuum pump
  6. customThe concentrates were purified by silica gel column chromatography
  7. washwashed by methanol

Quellen und Nachweise

ORD-Eintrag
ord-9385967d41c94830bc013193aab9291d
Quelldatensatz
uspto-grants-2012_06
Patentnummer
US08202633B2

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