反应详情

温度

80 °C

Triethylamine (1.5 mL, 11 mmol) and 2-chloro-N-ethylpyrimidine-5-carboxamide (830 mg, 4.47 mmol) were added sequentially to a solution of (S)-piperidin-3-ol hydrochloride (677 mg, 4.92 mmol) in acetonitrile (25 mL) at 20-25° C. The reaction mixture was heated to 80° C. for 16 hours. The mixture was then cooled to 20-25° C. and was concentrated under reduced pressure. The resulting residue was dissolved in EtOAc (25 mL) and washed with saturated NH4Cl (10 mL) and brine (10 mL). The organic phase was dried over Na2SO4, filtered, and concentrated to provide (S)—N-ethyl-2-(3-hydroxypiperidin-1-yl)pyrimidine-5-carboxamide (827 mg, 73%).

1. temperatureThe mixture was then cooled to 20-25° C.
2. concentrationwas concentrated under reduced pressure
3. dissolutionThe resulting residue was dissolved in EtOAc (25 mL)
4. washwashed with saturated NH4Cl (10 mL) and brine (10 mL)
5. dry with materialThe organic phase was dried over Na2SO4
6. filtrationfiltered
7. concentrationconcentrated