反应详情

N-[1-(2-Amino-benzoyl)-piperidin-4-yl]-N-cyclopropyl-3-trifluoromethyl-benzenesulfonamide (11) (0.170 g, 0.34 mmol) and pyridine (0.035 g, 0.45 mmol) was taken up in 1 ml of CHCl3. Chloroformic acid 2-chloroethyl ester (0.049 g, 0.34 mmol) was added over 5 minutes, and stirred at room temperature for 2 h. The reaction mixture was diluted with 30 ml of EtOAc and washed with 10 ml of H2O. The organic layer was dried over MgSO4 and concentrated to dryness. The crude product was purified through a column of silica gel with a gradient of 70% to 100% EtOAc in hexane to afford the title compound 12 (colorless amorphous, 152 mg, 83%). LC: 100%. MS: m/z=537.

1. washwashed with 10 ml of H2O
2. dry with materialThe organic layer was dried over MgSO4
3. concentrationconcentrated to dryness
4. customThe crude product was purified through a column of silica gel with a gradient of 70% to 100% EtOAc in hexane