反应详情

Trifluoromethanesulfonic anhydride (0.12 mL) was added to a flask charged with a stir bar, 1-cyclopropyl-4-hydroxy-1H-pyridin-2-one (0.10 g), NEt3 (0.24 mL), and dichloromethane (8 mL) and chilled in an ice/EtOH bath. The resulting mixture was stirred with cooling for 2 h and at ambient temperature for another 2 h. Then, the solution was diluted with dichloromethane and washed in succession with water, aqueous NaHCO3 solution, and water. The organic solution was dried (MgSO4), the solvent was removed, and the residue was purified by chromatography on silica gel (dichloromethane/methanol 99:1->90:10) to afford the title compound as a resin-like solid. Yield: 0.07 g (36% of theory). Mass spectrum (ESI+): m/z=284 [M+H]+.

1. additioncharged with a stir bar
2. washwashed in succession with water, aqueous NaHCO3 solution, and water
3. dry with materialThe organic solution was dried (MgSO4)
4. customthe solvent was removed
5. customthe residue was purified by chromatography on silica gel (dichloromethane/methanol 99:1->90:10)