反应详情

温度

90 °C

A vigorously stirred mixture of 5-bromo-3-fluoro-2-hydroxypyridine (440 mg, 2.3 mmol), 1-(2-chloroethyl)-1H-pyrazole (330 mg, 2.5 mmol) and K2CO3 (380 mg, 2.77 mmol) in DMF (5 mL) was heated to 90° C. for 16 h. After cooling to room temperature the solvent was removed in vacuo and the crude partitioned between water and EtOAc. The aqueous was extracted with EtOAc (×3) and the combined organics dried (MgSO4) and concentrated in vacuo. Purification by column chromatography (gradient: 20%-100% EtOAc in pet. ether 40-60) yielded (Intermediate 6) as a clear oil.

1. temperatureAfter cooling to room temperature the solvent
2. customwas removed in vacuo
3. customthe crude partitioned between water and EtOAc
4. extractionThe aqueous was extracted with EtOAc (×3)
5. dry with materialthe combined organics dried (MgSO4)
6. concentrationconcentrated in vacuo
7. customPurification by column chromatography (gradient: 20%-100% EtOAc in pet. ether 40-60)