反应详情

To a solution of EXAMPLE 443B (500 mg) in N,N-dimethylformamide (5 mL) was added NaH (65% in mineral oil, 252 mg) at room temperature. The mixture was stirred for 30 minutes, and then 5,6-dichloropyridine-3-sulfonamide (0.6 g) was added. The mixture was stirred at room temperature overnight. The mixture was poured over aqueous NH4Cl and extracted with ethyl acetate (3×100 mL). The combined organic layers were washed with water, brine and dried over Na2SO4. After filtration and evaporation of solvent, the residue was loaded on a silica gel cartridge and eluted with 30% ethyl acetate in hexane to provide the title compound.

1. stirringThe mixture was stirred at room temperature overnight
2. extractionextracted with ethyl acetate (3×100 mL)
3. washThe combined organic layers were washed with water, brine
4. dry with materialdried over Na2SO4
5. filtrationAfter filtration and evaporation of solvent
6. washeluted with 30% ethyl acetate in hexane