反应详情

温度

100 °C

In a microwave vial, 2-bromo-6-iodo-3-methoxypyridine (10-1 or 3-3, 150 mg, 0.48 mmol, 1 equiv) was dissolved in DMF (300 uL). Sodium ethoxide (268 uL, 21 wt % in EtOH, 0.72 mmol, 1.5 equiv) was added to the solution, and the reaction was heated in the microwave for 5 minutes at 100° C. The reaction mixture was partitioned between saturated NaHCO3 and DCM. The organic phase was washed once with brine, dried over Mg2SO4 and concentrated. The residue was purified by normal phase column chromatography (0-20% EtOAc in hexanes) to give the title compound (10-2). ESI+MS [M+H]+ C8H11INO2: 280.0 found, 280.1 required.

1. customThe reaction mixture was partitioned between saturated NaHCO3 and DCM
2. washThe organic phase was washed once with brine
3. dry with materialdried over Mg2SO4
4. concentrationconcentrated
5. customThe residue was purified by normal phase column chromatography (0-20% EtOAc in hexanes)