反应详情

温度

100 °C

A round-bottomed flask equipped with a reflux condenser was charged with 252a (200 mg, 0.64 mmol), (3-(acetoxymethyl)-2-(7,7-dimethyl-1-oxo-3,4,7,8-tetrahydro-1H-cyclopenta[4,5]pyrrolo[1,2-a]pyrazin-2(6H)-yl)pyridin-4-yl)boronic acid 199e (309 mg, 0.64 mmol), PdCl2(dppf) (52.5 mg, 0.060 mmol), K3PO4 (333 mg, 1.29 mmol), sodium acetate (105 mg, 1.29 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 in vacuo. The residue was purified by silica-gel column chromatography eluting with 1:20 methanol/dichloromethane to afford 252b as a yellow solid (120 mg, 27.6%). MS-ESI: [M+H]+ 584.3

1. customA 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 in vacuo
5. customThe residue was purified by silica-gel column chromatography
6. washeluting with 1:20 methanol/dichloromethane