反应详情

To a solution of 6-methyl-5-nitropyridin-2-ol (0.5 g, 3.2 mmol) in acetonitrile (10 mL) was added NaH (0.35 g, 8.64 mmol) and the reaction mixture was stirred for 15 minutes at room temperature. To the reaction mixture was added 2,2-difluoro-2-(fluoro-sulfonyl)acetic acid (1.1 mL, 5.5 mmol) dropwise. The reaction mixture was stirred for a further 15 minutes. The reaction mixture was then quenched by the addition of water, and diluted with EtOAc. The organic layer was washed with water and brine, dried over sodium sulphate and concentrated. The crude material obtained was purified by column chromatography (silica: 100-200 mesh, MeOH:DCM 2-4%) to afford the title compound (0.5 g, 75%) as a white solid. LCMS (ES−) 202.85 (M−H)−, RT 2.75 minutes (method 1).

1. stirringThe reaction mixture was stirred for a further 15 minutes
2. customThe reaction mixture was then quenched by the addition of water
3. additiondiluted with EtOAc
4. washThe organic layer was washed with water and brine
5. dry with materialdried over sodium sulphate
6. concentrationconcentrated
7. customThe crude material obtained
8. customwas purified by column chromatography (silica: 100-200 mesh, MeOH:DCM 2-4%)