反应详情

1-tert-butoxy-3-(bis(3,5-dimethylphenyl)phosphino)isoquinoline (0.96, 2.2 mmol) is dissolved in neat concentrated formic acid (9 mL), and the solution is stirred at ambient temperature for 1 hour. Precipitation of the isoquinolone was induced by dilution with H2O (25 mL), and the suspension is filtered through a glass frit. The white flakes are washed with 70% formic acid solution (3×5 mL). The combined aqueous formic acid filtrates are concentrated under reduced pressure, and the opaque residue is crystallized from acetone yielding 3-bis(3,5-dimethylphenyl)phosphino-2H-isoquinolin-1-one (0.55 g, 66%).

1. customPrecipitation of the isoquinolone
2. filtrationthe suspension is filtered through a glass frit
3. washThe white flakes are washed with 70% formic acid solution (3×5 mL)
4. concentrationThe combined aqueous formic acid filtrates are concentrated under reduced pressure
5. customthe opaque residue is crystallized from acetone