反应详情

温度

100 °C

A 100-mL single-neck round-bottomed flask was charged with 2-(6-tert-butyl-8-fluoro-1-oxophthalazin-2(1H)-yl)-4-chloronicotinaldehyde 103b (216 mg, 0.6 mmol), 3-(5-((2S,5R)-2,5-dimethyl-4-(oxetan-3-yl)piperazin-1-yl)pyridin-2-ylamino)-1-methyl-5-(4,4,5-trimethyl-1,3,2-dioxaborolan-2-yl)pyridin-2(1H)-one (360 mg, 0.72 mmol), Pd(dppf)Cl2 (30 mg, 0.03 mmol), K3PO4 (270 mg, 1.2 mmol), and NaOAc.3H2O (180 mg, 1.2 mmol) in CH3CN (80 mL). The system was evacuated and refilled with N2. The reaction mixture was heated at 100° C. 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 flash column chromatography eluting with 25:1 of CH2Cl2/MeOH to afford 110a (160 mg, 42%) as a yellow brown solid. MS: [M+H]+ 693.3.

1. customThe system was evacuated
2. additionrefilled with N2
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 flash column chromatography
7. washeluting with 25:1 of CH2Cl2/MeOH