反应详情

温度

60 °C

1-(5-Chloro-4-fluoro-2-hydroxy-3-iodophenyl)ethanone (13 g, 41 mmol) was dissolved in N,N-dimethylformamide (41.3 mL). Methyl iodide (3.9 mL, 62 mmol) was added followed by potassium carbonate (11 g, 83 mmol). The reaction was heated at 60° C. for 1 hour. The mixture was cooled to room temperature, diluted with ether. The organic layers were separated and combined, washed with water, dried over MgSO4, concentrated and purified on silica gel (eluting with 0 to 10% EtOAc in hexanes) to give the desired product (10 g, 70%). LCMS calculated for C9H8ClFIO2 (M+H)+: m/z=328.9; Found: 328.9.

1. temperatureThe mixture was cooled to room temperature
2. customThe organic layers were separated
3. washwashed with water
4. dry with materialdried over MgSO4
5. concentrationconcentrated
6. custompurified on silica gel (eluting with 0 to 10% EtOAc in hexanes)