反应详情

2-((1S,2R)-2-(piperidin-4-yl)cyclopropyl)ethanol (2.5 g, 14.77 mmol) was dissolved in DMF (30 ml) at RT under N2 and cesium carbonate (7.22 g, 22.15 mmol) was added. The mixture was stirred at RT for 5 min and 2-chloro-5-methoxypyrimidine (2.56 g, 17.72 mmol) was added. The mixture was stirred at 100° C. overnight. The mixture was diluted with EtOAc (100 ml), washed with sat. NH4Cl (100 ml), dried over MgSO4, and the volatiles evaporated under reduced pressure. The crude material was purified by silica gel column chromatography (100 g SNAP, 20˜60% EtOAc in hexane) to afford the titled compound. LC/MS (m/z): 278 (M+H)+. Rf was 0.4 @ 50% EtOAc in hexanes (blue spot on CAM stain).

1. stirringThe mixture was stirred at 100° C. overnight
2. washwashed with sat. NH4Cl (100 ml)
3. dry with materialdried over MgSO4
4. customthe volatiles evaporated under reduced pressure
5. customThe crude material was purified by silica gel column chromatography (100 g SNAP, 20˜60% EtOAc in hexane)