Reaktion #554567

ord-efba66156385427dbe80e4808b229765

Reaktionsgleichung

O=P(Cl)(Cl)Cl
Phosphorus oxychloride
CN(C)c1ccccc1
dimethylaniline
c1ccc2c(c1)cnc1ccccc12
phenanthridine
Clc1ccc2cnc3ccccc3c2c1
9-chlorophenanthridine
Ausbeute 96.0%

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturby refluxing for 3 hours
  2. 2
    Extraktionthe obtained solid was extracted with chloroform
  3. 3
    Trocknenby drying with sodium sulfate
  4. 4
    FiltrationAfter filtration
  5. 5
    Sonstigethe filtrate was evaporated to dryness under reduced pressure
  6. 6
    SonstigeThe obtained solid was purified by column chromatography (eluent: chloroform) (amount: 2.1 g, yield: 96%)

Vorschrift

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%).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08623239B2uspto-grants-2014_01