反应详情

A 50-mL round-bottomed flask equipped with a reflux condenser was charged with 119a (180 mg, 0.50 mmol), 3-(acetoxymethyl)-2-(6-tert-butyl-8-fluoro-1-oxophthalazin-2(1H)-yl)pyridine-4-ylboronic acid 116c (207 mg, 0.50 mmol), Pd(dppf)Cl2 (41 mg, 0.050 mmol), K3PO4 (212 mg, 1.0 mmol), sodium acetate (82 mg, 1.0 mmol), water (0.5 mL), and acetonitrile (10 mL). After three cycles of vacuum/argon flush, the mixture was heated at reflux for 2 h. It was then cooled to room temperature and filtered. The filtrate was concentrated under reduced pressure and the resulting residue was purified by silica-gel column chromatography eluting with 30:1 dichloromethane/methanol to afford 119b as a white solid (175 mg, 60%). MS-ESI: [M+H]+ 586.4

1. customA 50-mL round-bottomed flask equipped with a reflux condenser
2. customAfter three cycles of vacuum/argon flush
3. temperaturethe mixture was heated
4. temperatureat reflux for 2 h
5. filtrationfiltered
6. concentrationThe filtrate was concentrated under reduced pressure
7. customthe resulting residue was purified by silica-gel column chromatography
8. washeluting with 30:1 dichloromethane/methanol