反应详情

Slurry 2-(4-methyl-2-oxo-pentyl)-isoindole-1,3-dione (2.8 g, 11.4 mmol) in concentrated HCl (18 mL), glacial acetic acid (16 mL) and water (13 mL). Stir the mixture at reflux for 16 h. Cool to room temperature and pour the solution onto ice (25 mL). Filter off the solids, wash the filtrate with cold water (20 mL) and concentrate in vacuo to a solid. Recrystallize the solid in ethanol (15 mL) and diethyl ether (50 mL). Decant off the solvent and dry the white paste under reduced pressure to obtain the desired intermediate as a white solid (1.4 g, 81%).

1. temperatureat reflux for 16 h
2. additionpour the solution onto ice (25 mL)
3. filtrationFilter off the solids
4. washwash the filtrate with cold water (20 mL)
5. concentrationconcentrate in vacuo to a solid
6. customRecrystallize the solid in ethanol (15 mL)
7. customDecant off the solvent
8. customdry the white paste under reduced pressure