反应详情

温度

105 °C

A 25-mL single-neck round-bottomed flask equipped with a magnetic stirrer and reflux condenser was charged with 1,4-dioxane (8 mL), 108c (250 mg, 1.07 mmol), 5-(4-(oxetan-3-yl)piperazin-1-yl)pyridin-2-amine (252 mg, 1 mmol), and cesium carbonate (700 mg, 2 mmol). Xantphos (30 mg, 0.08 mmol) and Pd2(dba)3 (55 mg, 0.08 mmol) were added, and the reaction mixture was heated at 105° C. for 3 h. After this time the reaction was cooled to room temperature and filtered. The filtrate was concentrated under reduced pressure and the residue was purified by silica gel chromatography eluting with CH2Cl2/MeOH (20:1) to afford 108d (250 mg, 60%). MS: [M+H]+ 386.

1. customA 25-mL single-neck round-bottomed flask equipped with a magnetic stirrer
2. temperaturereflux condenser
3. temperatureAfter this time the reaction was cooled to room temperature
4. filtrationfiltered
5. concentrationThe filtrate was concentrated under reduced pressure
6. customthe residue was purified by silica gel chromatography
7. washeluting with CH2Cl2/MeOH (20:1)