反应详情

温度

60 °C

1-(5-Chloro-2-hydroxy-3-iodo-4-methylphenyl)ethanone (18.9 g, 60.9 mmol, from Example 60, Step 1) was dissolved in DMF (61 mL). Iodoethane (7.3 mL, 91 mmol) was added followed by potassium carbonate (17.0 g, 120 mmol). The reaction was heated at 60° C. for 1 hour. The mixture was cooled to room temperature, diluted with ether, washed with water, dried over MgSO4, concentrated. The resulting residue was purified on silica gel (eluting with 0 to 10% EtOAc in hexanes) to give the desired product (18.9 g, 91.7%). LCMS calculated for C11H13ClIO2 (M+H)+: m/z=339.0. found: 339.0.

1. temperatureThe mixture was cooled to room temperature
2. washwashed with water
3. dry with materialdried over MgSO4
4. concentrationconcentrated
5. customThe resulting residue was purified on silica gel (eluting with 0 to 10% EtOAc in hexanes)