反应详情

Potassium carbonate (1.40 g, 10.14 mmol) was added to a solution of 4-Methylphenyl 2,4,5-trifluorobenzoate (Preparation 12, 1.80 g, 6.76 mmol), 5-chloro-6-fluoropyridin-3-ol (1.05 g, 7.10 mmol) in DMSO and the mixture was stirred at room temperature for 18 hours. The reaction mixture was diluted in EtOAc (50 mL), washed with water (2×25 mL) and the organic layer dried over sodium sulfate, filtered, and concentrated in vacuo. The remaining crude was then purified by silica gel chromatography eluting with 10 to 50% EtOAc in heptane to afford the title compound (1.48 g, 56%):

1. washwashed with water (2×25 mL)
2. dry with materialthe organic layer dried over sodium sulfate
3. filtrationfiltered
4. concentrationconcentrated in vacuo
5. customThe remaining crude was then purified by silica gel chromatography
6. washeluting with 10 to 50% EtOAc in heptane