反应详情

温度

90 °C

To 2,6-difluoro-pyridine (49, 3.80 g, 33.0 mmol) in 20.0 mL of N-methylpyrrolidone, 4-chloro-benzylamine (50, 5.6 mL, 46.0 mmol) and N,N-diisopropylethylamine (10.0 mL, 57.4 mmol) were added. The reaction was stirred at 90° C. overnight, then poured into 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 25% ethyl acetate in hexane. Appropriate fractions were combined and the solvents removed under vacuum, and the resulting material was washed with ethyl acetate/hexane to provide the desired compound as a white solid (51, 5.30 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 25% ethyl acetate in hexane
7. customthe solvents removed under vacuum
8. washthe resulting material was washed with ethyl acetate/hexane