反应详情

温度

80 °C

To 6-fluoro-pyridin-2-ylamine (43, 1.50 g, 13.4 mmol) in 52.9 mL of acetonitrile, 5-fluoro-6-methoxy-pyridine-3-carbaldehyde (57, 2.00 g, 12.9 mmol), triethylsilane (10.6 mL, 66.3 mmol), and trifluoroacetic acid (5.3 mL, 69.0 mmol) were added. The reaction was stirred at 80° C. overnight, then concentrated under vacuum, combined with water and extracted with ethyl acetate. The organic layer was dried over sodium sulfate, filtered and the filtrate concentrated under vacuum. The resulting material was purified by silica gel column chromatography, eluting with 15-100% ethyl acetate in hexane. Appropriate fractions were combined and concentrated under vacuum to provide the desired compound as white solid (58, 3.21 g).

1. concentrationconcentrated under vacuum
2. extractionextracted with ethyl acetate
3. dry with materialThe organic layer was dried over sodium sulfate
4. filtrationfiltered
5. concentrationthe filtrate concentrated under vacuum
6. customThe resulting material was purified by silica gel column chromatography
7. washeluting with 15-100% ethyl acetate in hexane
8. concentrationconcentrated under vacuum