反应详情

温度

115 °C

N-Cyclopropyl-N-[1-(2-nitro-benzoyl)-piperidin-4-yl]-3-trifluoromethyl-benzenesulfonamide (10) (0.403 mg, 0.81 mmol) was taken up in 7 ml of toluene. To the mixture, Fe (0.230 mg, 4.1 mmol), NH4Cl (0.440 g, 8.2 mmol) and H2O (0.8 ml) was added. The reaction mixture was heated at 115° C. and stirred for 3 hours. The reaction mixture was diluted with 30 ml of EtOAc, then filtrated by Celite. The filtration was concentrated and dryness under reduced pressure. The crude product was purified through a column of silica gel with a gradient of 35% to 80% EtOAc in hexane to afford the title compound 11 (pale yellow solid, 335 mg, 88%). LC: 100%. MS: m/z=467.

1. filtrationfiltrated by Celite
2. filtrationThe filtration
3. concentrationwas concentrated
4. customThe crude product was purified through a column of silica gel with a gradient of 35% to 80% EtOAc in hexane