反应详情

温度

90 °C

Potassium carbonate (0.140 g, 1.01 mmol) was added to a stirred solution of N-(sec-butylsulfonyl)-2,4,5-trifluorobenzamide (Preparation 68, 0.090 g, 0.30 mmol) in DMSO (1 mL). After 10 minutes a solution of 5-chloro-6-methoxypyridin-3-ol (Preparation 77, 0.088 g, 0.51 mmol) in DMSO (2 mL) was added at room temperature. The mixture was heated at 90° C. for 72 hours. The reaction mixture was diluted with water (25 mL) and extracted with EtOAc (3×25 mL). The combined organics were washed with water (25 mL), dried over magnesium sulfate, filtered, evaporated in vacuo. The resulting crude product was purified by silica gel chromatography eluting with 0 to 66% EtOAc in heptane to yield the title compound (0.068 g):

1. extractionextracted with EtOAc (3×25 mL)
2. washThe combined organics were washed with water (25 mL)
3. dry with materialdried over magnesium sulfate
4. filtrationfiltered
5. customevaporated in vacuo
6. customThe resulting crude product was purified by silica gel chromatography
7. washeluting with 0 to 66% EtOAc in heptane