N,N-Dimethylaniline → 9-Chlorophenanthridine

HRID 467385Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 467385
P(Cl)(Cl)([Cl:3])=O.CN(C)C1C=CC=CC=1.[CH:15]1[C:28]2[C:19](=[N:20][CH:21]=[C:22]3[C:27]=2[CH:26]=[CH:25][CH:24]=[CH:23]3)[CH:18]=[CH:17][CH:16]=1>O>[Cl:3][C:25]1[CH:24]=[CH:23][C:22]2[C:27]([CH:26]=1)=[C:28]1[C:19]([CH:18]=[CH:17][CH:16]=[CH:15]1)=[N:20][CH:21]=2

Komponenten

5

Edukt 3

HCID 949N,N-DimethylanilineHCID 9189PhenanthridineHCID 24813Phosphorus oxychloride

Produkt 1

HCID 673172599-ChlorophenanthridineAusbeute 96 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

Phosphorus oxychloride (15 ml) and dimethylaniline (0.63 ml) were added to phenanthridine (2.0 g), followed by refluxing for 3 hours. The solution was poured into H2O to generate a solid, and the obtained solid was extracted with chloroform, followed by drying with sodium sulfate. After filtration, the filtrate was evaporated to dryness under reduced pressure. The obtained solid was purified by column chromatography (eluent: chloroform) (amount: 2.1 g, yield: 96%).

Aufarbeitung

  1. temperatureby refluxing for 3 hours
  2. extractionthe obtained solid was extracted with chloroform
  3. dry with materialby drying with sodium sulfate
  4. filtrationAfter filtration
  5. customthe filtrate was evaporated to dryness under reduced pressure
  6. customThe obtained solid was purified by column chromatography (eluent: chloroform) (amount: 2.1 g, yield: 96%)

Quellen und Nachweise

ORD-Eintrag
ord-efba66156385427dbe80e4808b229765
Quelldatensatz
uspto-grants-2014_01
Patentnummer
US08623239B2

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