反应详情

To a mixture of 2.3 g of 1-(3-methanesulfonyl-propyl)-piperidin-4-ylamine dihydrochloride, 2.7 g (0.0095 mole) of 4-amino-3-methoxy-benzoic acid benzotriazol-1-yl ester and 15 mL of dimethylformamide was added 4.0 g (0.0395 mole) of triethylamine. The mixture was stirred at room temperature for 20 hours, then diluted with 150 mL of dichloromethane. The mixture was washed twice with 100 mL of sodium bicarbonate, once with 50 mL of water, once with 50 mL of brine, dried over anhydrous sodium sulfate, filtered, and concentrated under reduced pressure. The residue was purified by silica gel chromatography, eluting with dichloromethane-methanol (gradient, 100:0-80:20) to give 2.0 g of 4-amino-N-[1-(3-methanesulfonyl-propyl)-piperidin-4-yl]-3-methoxy-benzamide.

1. washThe mixture was washed twice with 100 mL of sodium bicarbonate, once with 50 mL of water, once with 50 mL of brine
2. dry with materialdried over anhydrous sodium sulfate
3. filtrationfiltered
4. concentrationconcentrated under reduced pressure
5. customThe residue was purified by silica gel chromatography
6. washeluting with dichloromethane-methanol (gradient, 100:0-80:20)