反应详情

温度

100 °C

A 50-mL round-bottomed flask equipped with a magnetic stirrer and a reflux condenser was charged with 123c (151 mg, 0.51 mmol), 3-(acetoxymethyl)-2-(6-tert-butyl-8-fluoro-1-oxophthalazin-2(1H)-yl)pyridin-4-ylboronic acid 116c (206 mg, 0.50 mmol), PdCl2(dppf) (22 mg, 0.030 mmol), K3PO4 (216 mg, 1.02 mmol), sodium acetate (84 mg, 1.02 mmol), acetonitrile (10 mL), and water (0.5 mL). After three cycles of vacuum/argon flush, the mixture was heated at 100° C. for 3 h. It was then filtered and the filtrate was evaporated under reduced pressure. The residue was purified by silica-gel column chromatography eluting with 1:3 petroleum/ethyl acetate to afford 123d as a yellow solid (158 mg, 53%). MS-ESI: [M+H]+ 587.2

1. customA 50-mL round-bottomed flask equipped with a magnetic stirrer and 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 1:3 petroleum/ethyl acetate