反应详情

温度

80 °C

To {5-[(5-bromo-1H-pyrrolo[2,3-b]pyridin-3-yl)-methoxy-methyl]-pyridin-2-yl}-(6-methoxy-pyridin-3-ylmethyl)-carbamic acid tert-butyl ester (154, 0.35 g, 0.63 mmol) in 20.0 mL of acetonitrile, triethylsilane (1.0 mL, 6.3 mmol) and trifluoroacetic acid (0.50 mL, 6.5 mmol) were added and the reaction stirred at 80° C. for 4 hours. The reaction was concentrated under vacuum and combined with aqueous potassium carbonate and extracted with ethyl acetate. The organic layer was filtered and the filtrate concentrated under vacuum. The resulting material was purified by silica gel column chromatography eluting with 20-100% ethyl acetate in hexane. Appropriate fractions were combined and concentrated under vacuum to provide the desired compound (P-2017, 165.1 mg). MS (ESI) [M+H+]+=423.8, 425.8

1. concentrationThe reaction was concentrated under vacuum
2. extractionextracted with ethyl acetate
3. filtrationThe organic layer was filtered
4. concentrationthe filtrate concentrated under vacuum
5. customThe resulting material was purified by silica gel column chromatography
6. washeluting with 20-100% ethyl acetate in hexane
7. concentrationconcentrated under vacuum