反应详情

A solution of the product of N-[2-(4-benzylpiperazin-1-yl)phenyl]methanesulfonamide (2.83 g, 8.2 mmol) in methanol (40 mL) was purged with nitrogen (0.25 hour). Ammonium formate (1.55 g, 24.6 mmol), formic acid (0.31 mL, 8.21 mmol) and palladium on activated charcoal (0.5 g) were added. The mixture was heated at reflux for 2 h., cooled, filtered, and the solvent was evaporated under reduced pressure. The residue was diluted with ethyl acetate and washed with aqueous potassium carbonate (saturated, 3×). The organic layer was dried (MgSO4) and the solvent was evaporated under reduced pressure to give the title compound as a pale yellow crystalline solid (1.196 g, 57%), δH (250 MHz, CDCl3) 7.52 (1H, dd, J 1.6, 8.0 Hz), 7.23-7.05 (4H, m), 3.06 (3H, s), 3.06-3.02 (4H, m), 2.85-2.78 (4H, m), and 1.80 (1H, br s).

1. temperatureThe mixture was heated
2. temperatureat reflux for 2 h.
3. temperaturecooled
4. filtrationfiltered
5. customthe solvent was evaporated under reduced pressure
6. additionThe residue was diluted with ethyl acetate
7. washwashed with aqueous potassium carbonate (saturated, 3×)
8. dry with materialThe organic layer was dried (MgSO4)
9. customthe solvent was evaporated under reduced pressure