Reaction #554567

Reaction equation

Phosphorus oxychloride

dimethylaniline

phenanthridine

→

9-chlorophenanthridine

Yield 96.0%

Solvents

H2O

Conditions

Workup

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

Procedure

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