反应详情

温度

60 °C

A mixture of 1-(3-bromo-5-chloro-4-fluoro-2-hydroxyphenyl)ethanone (4.8 g, 18 mmol), potassium carbonate (6.5 g, 47 mmol) and methyl iodide (2.5 mL, 40 mmol) in DMF (10 mL) was heated at 60° C. for 1 hour. The mixture was diluted with water and extracted with EtOAc. The combined organic layers were washed with brine, dried over sodium sulfate, and evaporated. The residue was purified on silica gel, eluting with 0 to 20% EtOAc in hexane, to yield the desired compound (2.2 g, 44%). LCMS calculated for C9H8BrClFO2 (M+H)+: m/z=280.9, 282.9. found: 281.0, 283.0.

1. extractionextracted with EtOAc
2. washThe combined organic layers were washed with brine
3. dry with materialdried over sodium sulfate
4. customevaporated
5. customThe residue was purified on silica gel
6. washeluting with 0 to 20% EtOAc in hexane