反应详情

温度

65 °C

2-((1S,2R)-2-(piperidin-4-yl)cyclopropyl)ethanol (810 mg, 4.79 mmol) and 2-(2-chloropyrimidin-5-yl)propan-2-ol (991 mg, 5.74 mmol) were dissolved in 12 mL of DMF, to which was added cesium carbonate (2.0 g, 6.20 mmol). The mixture was heated at 65° C. overnight. The mixture was cooled to rt, diluted with 20 mL of EtOAc and 20 mL of water. The layers were separated and the aqueous phase extracted with EtOAc (20 mL×2). The combined organic layers were dried over MgSO4, filtered, and concentrated under reduced pressure. The residue was purified by column chromatography on silica gel (KP-Sil 50 SNAP column, Biotage system) eluting with a range of 40-90% EtOAc/Hex over 12 CV to give the desired compound. LC/MS (m/z): 306 (M+H)+.

1. temperatureThe mixture was cooled to rt
2. customThe layers were separated
3. extractionthe aqueous phase extracted with EtOAc (20 mL×2)
4. dry with materialThe combined organic layers were dried over MgSO4
5. filtrationfiltered
6. concentrationconcentrated under reduced pressure
7. customThe residue was purified by column chromatography on silica gel (KP-Sil 50 SNAP column, Biotage system)
8. washeluting with a range of 40-90% EtOAc/Hex over 12 CV