反应详情

The above 2,9-di-t-butylphenanthridinone (3.0 g, 9.7 mmole) was added to a reaction flask containing phosphorus pentachloride (3.0 g, 14.6 mmole) and 50 mL of phosphoryl chloride. The reaction mixture was refluxed overnight, cooled to room temperature and diluted with toluene. The excess phosphoryl chloride and toluene were removed by a rotary evaporator. The residue was dissolved into ethyl acetate and washed with distilled water followed by brine. The solvent layer was dried over magnesium sulfate, filtered and concentrated to give the desired 2,9-di-tert-butyl-6-chlorophenanthridine (3.0 grams, 98%) as an off white solid. The product was confirmed by GC Mass Spec and not purified further but used directly in the next step.

1. temperatureThe reaction mixture was refluxed overnight
2. customThe excess phosphoryl chloride and toluene were removed by a rotary evaporator
3. dissolutionThe residue was dissolved into ethyl acetate
4. washwashed with distilled water
5. dry with materialThe solvent layer was dried over magnesium sulfate
6. filtrationfiltered
7. concentrationconcentrated