反应详情

温度

100 °C

A 100-mL flask equipped with a reflux condenser was charged with 147c (285 mg, 0.81 mmol), 3-(acetoxymethyl)-2-(6-tert-butyl-8-fluoro-1-oxophthalazin-2(1H)-yl)pyridin-4-ylboronic acid 116c (669 mg, 1.62 mmol), Pd(dppf)Cl2 (66.2 mg, 0.081 mmol), K3PO4 (343.4 mg, 1.62 mmol), sodium acetate (132.8 mg, 1.62 mmol), water (0.5 mL), and acetonitrile (15 mL). After three cycles of vacuum/argon flush, the mixture was heated at 100° C. for 3 hrs. 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 dichloromethane/methanol (50:1 to 30:1) to afford 147d as a brown solid (140.0 mg, 27%). MS-ESI: [M+H]+ 640.3.

1. customA 100-mL flask equipped with a reflux condenser
2. customAfter three cycles of vacuum/argon flush
3. temperatureIt was then cooled to room temperature
4. filtrationfiltered
5. concentrationThe filtrate was concentrated under reduced pressure
6. customthe resulting residue was purified by silica-gel column chromatography
7. washeluting with dichloromethane/methanol (50:1 to 30:1)