反应详情

A mixture of 1-(5-chloro-2-hydroxy-3-iodo-4-methylphenyl)ethanone (10 g, 32 mmol), dimethyl sulfate (3.7 mL, 39 mmol) and potassium carbonate (8.9 g, 64 mmol) in acetone (200 mL) was heated at reflux overnight. After evaporation to dryness, the mixture was diluted with water and extracted with ethyl acetate. The combined organic layers were washed with brine, dried over sodium sulfate, filtered 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 (8.99 g, 86%). LCMS calculated for C10H11ClIO2 (M+H)+: m/z=324.9. found: 324.9.

1. temperaturewas heated
2. temperatureat reflux overnight
3. customAfter evaporation to dryness
4. additionthe mixture was diluted with water
5. extractionextracted with ethyl acetate
6. washThe combined organic layers were washed with brine
7. dry with materialdried over sodium sulfate
8. filtrationfiltered
9. customevaporated to dryness
10. customThe residue was purified on silica gel
11. washeluting with 0 to 20% ethyl acetate in hexane