反应详情

温度

60 °C

A mixture of 1-(3-bromo-5-chloro-4-fluoro-2-hydroxyphenyl)ethanone (5.3 g, 20 mmol), potassium carbonate (7.2 g, 52 mmol) and methyl iodide (2.7 mL, 44 mmol) in N,N-dimethylformamide (20 mL) was heated at 60° C. for 1 hour. The mixture was filtered and washed with ethyl acetate. The filtrate was diluted with water and extracted with ethyl acetate. The combined organic layers were washed with brine, dried over sodium sulfate, and evaporated to dryness. The residue was purified on silica gel, eluting with 0 to 20% ethyl acetate in hexane, to yield the desired product (39% yield). LCMS calculated for C9H8BrClFO2 (M+H)+: m/z=280.9, 282.9. found: 280.8, 282.8.

1. filtrationThe mixture was filtered
2. washwashed with ethyl acetate
3. additionThe filtrate was diluted with water
4. extractionextracted with ethyl acetate
5. washThe combined organic layers were washed with brine
6. dry with materialdried over sodium sulfate
7. customevaporated to dryness
8. customThe residue was purified on silica gel
9. washeluting with 0 to 20% ethyl acetate in hexane