Réaction #554567

ord-efba66156385427dbe80e4808b229765

Équation de réaction

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

Solvants

Conditions de réaction

Conditions détaillées
See reaction.notes.procedure_details.

Traitement

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

Mode opératoire

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%).

Source

DOI: 10.6084/m9.figshare.5104873.v1Brevet: US08623239B2uspto-grants-2014_01