反应详情

To a stirred suspension of 222a (47 mg, 0.25 mmol) in acetonitrile (10 mL) and pyridine (20 uL) was added 4-acetamidobenzoyl chloride (49 mg, 0.25 mmol) in acetonitrile (1 mL) at 0° C. for 15 min. The reaction mixture was warmed up to room temperature and stirred for 4 hours, concentrated under reduced pressure. The crude was diluted in DCM and washed with NaHCO3 and brine. The organic layer was dried with Na2SO4 and evaporated. The residue was purified by flash chromatography on silica gel, eluents hexane-EtOAc (1:3), then EtOAc (100%) to afford the title compounds 223 (3 mg, 4% yield) and 224a (5 mg, 5% yield).

1. concentrationconcentrated under reduced pressure
2. additionThe crude was diluted in DCM
3. washwashed with NaHCO3 and brine
4. dry with materialThe organic layer was dried with Na2SO4
5. customevaporated
6. customThe residue was purified by flash chromatography on silica gel, eluents hexane-EtOAc (1:3)