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温度

0 °C

A suspension of 3-fluoro-2-hydroxypyridine (1 g, 8.8 mmol) in dry DMF (11 mL) was cooled in an ice bath. Bromine (1.55 g, 9.7 mmol) was added drop-wise over a period of 10 min and the reaction mixture stirred at 0° C. for 1 h then allowed to warm to room temperature and stirred for an additional 2 h. The reaction was quenched with water. The aqueous was extracted with DCM (×4) and the combined organics dried (MgSO4) and concentrated in vacuo. Purification by column chromatography (gradient: 20-100% EtOAc in pet. ether 40-60) yielded 5-Bromo-3-fluoro-2-hydroxypyridine as a pale yellow solid.

1. temperaturewas cooled in an ice bath
2. temperatureto warm to room temperature
3. stirringstirred for an additional 2 h
4. customThe reaction was quenched with water
5. extractionThe aqueous was extracted with DCM (×4)
6. dry with materialthe combined organics dried (MgSO4)
7. concentrationconcentrated in vacuo
8. customPurification by column chromatography (gradient: 20-100% EtOAc in pet. ether 40-60)