Reacción #554567

ord-efba66156385427dbe80e4808b229765

Ecuación de reacción

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

Disolventes

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    Temperaturaby refluxing for 3 hours
  2. 2
    Extracciónthe obtained solid was extracted with chloroform
  3. 3
    Secadoby drying with sodium sulfate
  4. 4
    FiltraciónAfter filtration
  5. 5
    Otrothe filtrate was evaporated to dryness under reduced pressure
  6. 6
    OtroThe obtained solid was purified by column chromatography (eluent: chloroform) (amount: 2.1 g, yield: 96%)

Procedimiento

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%).

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US08623239B2uspto-grants-2014_01