反应详情

To a stirred solution of 1-(5-chloro-4-fluoro-2-hydroxyphenyl)ethanone (8.0 g, 42 mmol) in acetic acid (80 mL) was added N-bromosuccinimide (9.0 g, 50 mmol) and the resulting mixture was stirred at room temperature for 18 hours. The reaction mixture was concentrated, neutralized with saturated sodium bicarbonate solution and extracted with EtOAc. The combined organic layers were washed with brine, dried over sodium sulfate, and then concentrated to dryness under reduced pressure. The residue was purified on silica gel, eluting with 0 to 20% EtOAc in hexane, to yield the desired product (10.5 g, 93%). LCMS calculated for C8H6BrClFO2 (M+H)+: m/z=266.9, 268.9. found: 267.1, 269.1.

1. concentrationThe reaction mixture was concentrated
2. extractionextracted with EtOAc
3. washThe combined organic layers were washed with brine
4. dry with materialdried over sodium sulfate
5. concentrationconcentrated to dryness under reduced pressure
6. customThe residue was purified on silica gel
7. washeluting with 0 to 20% EtOAc in hexane