反应详情

温度

100 °C

A 50-mL round-bottomed flask equipped with a reflux condenser was charged with 5-bromo-1-methyl-3-(5-methyl-1H-pyrazol-3-ylamino)pyridin-2(1H)-one 118a (142 mg, 0.50 mmol), 3-(acetoxymethyl)-2-(6-tert-butyl-8-fluoro-1-oxophthalazin-2(1H)-yl)pyridin-4-ylboronic acid 116c (310 mg, 0.75 mmol), Pd(dppf)Cl2 (18 mg, 0.025 mmol), K3PO4 (212 mg, 1.0 mmol), sodium acetate (82 mg, 1.0 mmol), acetonitrile (10 mL), and water (0.2 mL). After three cycles of vacuum/argon flush, the mixture was heated at 100° C. for 2 h. It was then filtered and the filtrate was evaporated under reduced pressure. The residue was purified by silica-gel column chromatography eluting with 25:1 dichloromethane/methanol to afford 121a as a brown solid (100 mg, 35%). MS-ESI: [M+H]+ 572.3

1. customA 50-mL round-bottomed flask equipped with a reflux condenser
2. customAfter three cycles of vacuum/argon flush
3. filtrationIt was then filtered
4. customthe filtrate was evaporated under reduced pressure
5. customThe residue was purified by silica-gel column chromatography
6. washeluting with 25:1 dichloromethane/methanol