反应详情

To a solution of 4-fluoro-3-nitrobenzenesulfonamide (1.26 g) and 1-cyclopropylpiperidin-4-amine (0.802 g) in tetrahydrofuran (20 mL) was added N,N-diisopropylethylamine (2.22 g) and 4-dimethylaminopyridine (35 mg). The mixture was stirred at reflux overnight. The mixture was diluted with ethyl acetate (200 mL) and washed with aqueous NaHCO3, water, and brine and dried over Na2SO4. After filtration and concentration, the residue was dissolved in dichloromethane and loaded on a column and eluted with dichloromethane (500 mL), 5% 7N NH3 in 10% methanol in dichloromethane (1.5 L) to give the product.

1. temperatureat reflux overnight
2. washwashed with aqueous NaHCO3, water, and brine
3. dry with materialdried over Na2SO4
4. filtrationAfter filtration and concentration
5. dissolutionthe residue was dissolved in dichloromethane
6. washeluted with dichloromethane (500 mL), 5% 7N NH3 in 10% methanol in dichloromethane (1.5 L)
7. customto give the product