反应详情

To (5-fluoro-6-methoxy-pyridin-3-ylmethyl)-(6-fluoro-pyridin-2-yl)-amine (58, 3.21 g, 12.8 mmol) in 100 mL of acetonitrile, N-bromosuccinimide (2.30 g, 12.9 mmol) in 30 mL of acetonitrile was added slowly at room temperature. The reaction was stirred at room temperature for 4 hours, then poured into aqueous potassium carbonate 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 20% ethyl acetate in hexane. Appropriate fractions were combined and concentrated under vacuum to provide the desired compound (59, 3.60 g).

1. extractionextracted with ethyl acetate
2. dry with materialThe organic layer was dried over sodium sulfate
3. filtrationfiltered
4. concentrationthe filtrate concentrated under vacuum
5. customThe resulting material was purified by silica gel column chromatography
6. washeluting with 20% ethyl acetate in hexane
7. concentrationconcentrated under vacuum