反应详情

A solution of 2-bromo-5-methyl-pyridin-3-ylamine (1 g, 5.38 mmol) and 4-chloro-3-trifluoromethylbenzenesulfonylchloride (1.8 g, 6.46 mmol) in pyridine (5 mL) was stirred at 60° C. for 12 h. The mixture was concentrated under reduced pressure and to it, was added 1:1 EtOAc-10% aqueous HCl (50 mL). Aqueous layer was separated and extracted with EtOAc (2×50 mL). Combined EtOAc layers were washed with 10% aqueous HCl (50 mL), dried (anhydrous Na2SO4), concentrated and column purified (SiO2, 50% EtOAc-hexanes) to obtain N-(2-bromo-5-methyl-pyridin-3-yl)-4-chloro-3-trifluoromethyl-benzenesulfonamide (1.42 g) in 84% yield as a half white solid. ESMS m/z (relative intensity): 429 (M+H)+ (100).

1. concentrationThe mixture was concentrated under reduced pressure and to it
2. additionwas added 1:1 EtOAc-10% aqueous HCl (50 mL)
3. customAqueous layer was separated
4. extractionextracted with EtOAc (2×50 mL)
5. washCombined EtOAc layers were washed with 10% aqueous HCl (50 mL)
6. dry with materialdried (anhydrous Na2SO4)
7. concentrationconcentrated
8. customcolumn purified (SiO2, 50% EtOAc-hexanes)