反应详情

温度

120 °C

A solution of N-(4-iodo-6-methoxypyridin-3-yl)pivalamide (Compound 2, 2.33 g, 7.0 mmol) in 10% H2SO4 (70 ml) was heated to reflux at 120° C. for 5 h. The mixture was cooled to 0° C. and was quenched cautiously with solid NaOH (10 g), extracted with EtOAc (×2). The combined organic layer was washed with brine, dried over Na2SO4, and concentrated in vacuo. The residue was purified by chromatography on silica gel (0→30% EtOAc-hexanes) to yield the title compound as off-white solid.

1. temperatureThe mixture was cooled to 0° C.
2. customwas quenched cautiously with solid NaOH (10 g)
3. extractionextracted with EtOAc (×2)
4. washThe combined organic layer was washed with brine
5. dry with materialdried over Na2SO4
6. concentrationconcentrated in vacuo
7. customThe residue was purified by chromatography on silica gel (0→30% EtOAc-hexanes)